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Economical and Environmentally Friendly Track of Biowaste

Recycling of Scallop Shells to Calcium Lactate
Somkiat Seesanong, Yok Wongchompoo, Banjong Boonchom,* Chuchai Sronsri, Nongnuch Laohavisuti,
Kittichai Chaiseeda,* and Wimonmat Boonmee

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ABSTRACT: The scallop shell waste (Pectinidae, one of saltwater clams) was used as a raw material (precursor) to prepare calcium
lactate (Ca(C2H4OHCOO)2), and the physicochemical properties of scallop-derived calcium lactate were then investigated. The
scallop waste was first ground to obtain calcium carbonate (CaCO3) powder, and the calcium lactate compounds were successfully
synthesized by the reactions between shell-derived CaCO3 and lactic acid (C2H4OHCOOH). The short preparation time, high
percentage yield, and low-cost production are the preferred manners, and, in this research, it was the reaction of 70 wt % lactic acid
and scallop-derived CaCO3. The thermal decompositions of both CaCO3 precursor and all prepared calcium lactates resulted in the
formation of calcium oxide (CaO), which is widely used as a catalyst for biodiesel production. By comparing with the literature, the
results obtained from the characterization instruments (infrared spectrophotometer, X-ray diffractometer, thermogravimetric
analyzer, and scanning electron microscope) confirmed the formation and crystal structure of both CaCO3 and its calcium lactate
product. The morphologies of calcium lactate show different sizes depending on the acid concentration used in the reaction process.
Consequently, this work reports an easy, uncomplicated, low-cost technique to change the cheap calcium compound product
(scallop CaCO3) derived from shellfish waste to the valuable compound (calcium lactate), which can be used in many industries.

1. INTRODUCTION processes3 and can also add valuable revenue-generating

Economic, social, and environmental sustainability is the most streams through mass material production.
important for future globalization. Moreover, sustainable Aquaculture is an important occupation in many countries.
development is the development that is in line with the It is widely designed to manage and control the organisms
needs of both the present and the future.1 Nowadays, the from both freshwater and marine sources.4 The three main
development and commercialization of utilizing products aqua-cultured animals, i.e., fish, shrimp, and shellfish farms, are
obtained from biowaste materials are significantly increasing. an essential protein source of both humans and other
Abundant and especially low-cost waste matter and its organisms. Shellfish production, especially bivalve shellfish,
chemical conversion to useful compounds are key points in represents the main segment of the global seafood industry.
the broad field of green chemistry. In addition, the recycling of
various biowastes is in line with many developing and
developed countries to solve the environmental issues of the Received: January 6, 2022
wastes, especially in Thailand where the bio-circular-green Accepted: April 8, 2022
(BCG) economical model was established to change wastes to Published: April 25, 2022
valuable products.2 Transformation of biowaste materials into
value-added products shows a significant regional impact
through the reduction of biowaste and biowaste treatment
© 2022 The Authors. Published by
American Chemical Society https://doi.org/10.1021/acsomega.2c00112
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Table 1. Preparation Conditions, Percentage Yields, and Production Cost of Calcium Lactate (CaLT) Monohydrate
(Ca(C2H4OHCOO)2·H2O) Produced from the Reaction between Scallop-Derived CaCO3 Powders and Various Lactic Acid
Concentrations
compound lactic acid concentration (wt %) percentage yield (%) dried time reaction temperature (°C) production cost (USD·kg−1)
CaLT-40 40 92.68 3h 36 0.1405
CaLT-50 50 93.49 2h 47 0.1390
CaLT-60 60 89.86 45 min 57 0.1390
CaLT-70 70 90.49 0.30 min 64 0.1366

Shellfish industries can be found in all coastal regions of many additive with E number of E327 classified by the United States
countries. Scallop is one of the well-known shellfishes, which is Food and Drug Administration (U.S. FDA) as Generally
widely distributed throughout the world.5 Scallop aquaculture Recognized as Safe (GRAS),20 for uses as a stabilizer and
is one of the great economic importance, which supports both thickener, nutritional supplement, leavening agent, flavor
maricultural efforts and commercial fisheries. According to the enhancer or flavoring agent, and firming agent.21 For plant
National Oceanic and Atmospheric Administration (NOAA) and animal industries, it has been applied as a calcium source
Fisheries, about 23 000 tons of commercial landings of Atlantic for animals and plants and used to maintain and extend the
Sea were observed in 2020 with the value of about 490 million shelf life of flowers, fruits, and vegetables.22 For environmental
USD. The information reported by the Food and Agriculture industries, it is a coagulant for removing suspended solids from
Organization of the United Nations (FAO) Fisheries and water23 because it is a renewable, nontoxic, and biodegradable
Aquaculture Department showed that more than 2 million tons compound.24 For chemical industries, it was used as a raw
of scallops have been consumed per year.6 However, the edible material for the production of advanced compounds such as
part of the scallop had only 10−16 wt %, resulting in about lactic acid (C2H4OHCOOH) to use in food and medical
84−90 wt % of scallop waste.7 This scallop food industry fields,25 and calcium oxide (CaO) to use as a catalyst.26 For
makes millions of tons of shellfish’s byproducts, which can be construction industries, it is mixed into the concrete to
considered an interesting biowaste resource.8 The disposal of increase the compressive strength and reduce the water
scallop shell wastes is turning into an increasingly serious issue permeability, resulting in the formation of efficient bio-
for the marine aquaculture industries and various consumer concrete.27 Because of the large applications of calcium lactate
countries. described above, consequently, it had been prepared by many
Large numbers of shell wastes are conventionally dumped preparation methods using starting agents such as lactic acid
into landfills and/or public waters, which cause many with nonrenewable ores such as calcium carbonate (CaCO3)
environmental problems including health and sanitation issues, and calcium hydroxide (Ca(OH)2).
damage of the natural landscape, unpleasant smell as a The transformations of the shellfish wastes were recom-
consequence of the decomposition of organics attached to mended by the BCG model2 to transform waste into valuable
the shells, and management of public water surface as well as calcium compounds such as calcium acetate and calcium
pollution to coastal fisheries.9−11 Consequently, some green lactate. Simple and rapid processes were also suggested in
technologies are required to find the methods to reduce the waste recycling. Recently, the recycling of biowastes is the
above-mentioned problems.12 For example, Borić et al. strong intention. For example, crab shell,28 eggshells,29
presented a sustainable and feasible platform for the extraction littleneck clam (Ruditapes philippinarum) shell,30 and butter
and purification of chitin (the second most abundant natural clam (Saxidomus purpuratus) shell31 were used as starting
polysaccharide, after cellulose) from crustacean waste. Chitin agents to synthesize calcium lactate. The difference in starting
was isolated from crustacean waste using a hybrid deminer- agents and preparation methods are the effects of the different
alization/dielectric barrier discharge (DBD) plasma process. physicochemical properties of the calcium lactate products. A
Plasma and organic acids were applied to remove protein and large number of restaurants and many marine product
inorganic minerals from the waste, respectively.13,14 Moreover, manufacturers along Thailand’s coast discharge scallop shell
Bradić et al. presented a sustainable process for the recovery of as a waste, resulting in the increase of processing cost to
value-added biomaterials from the abundant shrimp shell waste exterminate the scallop waste.32
using natural deep eutectic solvents. Due to the properties of CaCO3 is the main composition (98 wt %) of scallop with
the selected solvent, chitin (98% purity) was separated from some small interferences, which are magnesium carbonate
minerals and proteins in a single step.15 (MgCO3, 0.79 wt %) and strontium carbonate (SrCO3, 0.15 wt
Calcium lactate, a white crystal salt with formula C6H10CaO6 %).33 Therefore, scallop shell was considered a suitable raw
or Ca(C2H4OHCOO)2, is composed of two lactate anions material for the production of calcium lactate. The objective of
(CH3CHOHCO2−) for each calcium cation (Ca2+). It is this work is to synthesize calcium lactate through a low-cost,
available in several hydrate forms, and calcium lactate rapid, and simple process using scallop shell as the precursor.
pentahydrate (C6H10CaO6·5H2O) is the most common one. The natural form of scallop shell was first cleaned and milled to
Calcium lactate has been extensively applied in many obtain the scallop-derived CaCO3 powder. After that, the
industries. For medicine industries, it has been applied in reaction between scallop-derived CaCO3 powder with lactic
humans and other organisms such as an antidote for soluble acid was employed to prepare the calcium lactate. The
fluoride ingestion,16 hypocalcemia (calcium deficiencies),17 difference in the synthesis conditions may influence the
oral calcium administration for prevention of tetany, anti-tartar characteristics of the synthesized product. Therefore, the effect
agent in some mouthwashes and toothpaste, antacid,18 and of some operational parameters, i.e., the concentration of lactic
calcium source for preventing and treating calcium deficien- acid used in the synthesis process, on the percentage yield,
cies.19 For food industries, it has been applied as a food drying time, reaction temperature, and other physicochemical
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Table 2. Chemical Compositions and Purities of Raw-CaCO3 Starting Material and Scallop-Derived Calcium Lactate (CaLT)
Prepared at Different Lactic Acid Concentrations
compound chemical composition (%) purity (%)
CaO O Na Mg S P K summation
CaCO3 69.92 27.5 0.14 0.59 0.25 1.6 100 97.88
CaLT-40 70.20 29.2 0.61 100 98.27
CaLT-50 70.04 29.3 0.66 100 98.06
CaLT-60 69.56 28.2 0.83 0.24 0.82 0.36 100 97.38
CaLT-70 70.88 26.5 0.54 0.45 1.63 100 99.23

properties of calcium lactate, were also investigated. All transform infrared (FTIR) spectrophotometry results. For the
investigated parameters were then used to point out and elemental quantities of calcium and oxygen contents in calcium
obtain the suitable parametric value that synthesizes a low-cost lactate products, the theoretical values are 71.43% CaO and
calcium lactate product. Scallop-derived CaCO3 powder and all 28.57% O, which are close to the observed values of all
synthesized calcium lactate products were analyzed by several synthesized calcium lactate products. Based on elemental
scientific methods including X-ray fluorescence (XRF), X-ray content, the purities of calcium lactates were estimated and
diffraction (XRD), infrared (IR) adsorption, thermogravim- found to be in the range of 97.38−99.23%. The highest
etry/derivative thermogravimetry (TG/DTG), and scanning amount of the elemental impurities was observed in CaLT-60
electron microscopy (SEM) to prove that the obtained target followed by CaLT-40. Nevertheless, the accumulation of toxic
compounds were CaCO3 and calcium lactate. elements in scallop shells may occur depending on the source.
Therefore, the elemental compositions should be investigated
2. RESULTS AND DISCUSSION before each use. According to the results, calcium lactates
2.1. Production Results. Table 1 illustrates the prepara- derived from scallop shell waste obtained in this work did not
tion conditions, percentage yields, and production cost of have the contents of toxic elements such as chromium (Cr),
calcium lactate monohydrate (Ca(C2H4OHCOO)2·H2O) strontium (Sr), cadmium (Cd), arsenic (As), lead (Pb),
produced from the reaction between scallop-derived CaCO3 chlorine (Cl), fluorine (F), etc. From the obtained XRF data,
and various lactic acid concentrations. They show an increase the lowest amount of impurities was observed from the CaLT-
in the temperature of the exothermic reaction as the 70 sample, pointing out that the lactic acid with a
concentration of lactic acid increases. These reaction temper- concentration of 70 wt % should be used as the reagent to
atures are the highest temperature that occurred during the prepare calcium lactate with the highest purity.
reaction. As described in Section 4.2, the preparation of 2.3. Thermal Analysis. A PerkinElmer Pyris Diamond
calcium lactate using higher concentrations of lactic acid leads TGA instrument was applied to confirm the identity of calcium
to the completely dried powder within a short time. For carbonate (CaCO3) obtained from the scallop shell waste and
example, completely dried powders were obtained at the its calcium lactate monohydrate (Ca(C2H4OHCOO)2·H2O)
exposure time of about 3 h for CaLT-40, but for CaLT-70, it products. The TG and DTG curves as presented in Figure 1
took only 30 min. The percentage yields of the calcium lactate
product obtained from four reactions were found in the range
of 89−93%, which were not significantly different, with the
highest production yield observed when 50 wt % lactic acid
was employed to prepare calcium lactate. The cost of the
production process with consideration of only raw materials for
every four reactions was found to be closely same (0.1366−
0.1405 USD·kg−1). In terms of production results, short
preparation time, high percentage yield, and low production
cost are the preferred characteristics, and, in this research, it
was the reaction between 70 wt % lactic acid and scallop-
derived CaCO3 labeled as CaLT-70.
2.2. X-ray Fluorescence. A Bruker SRS 3400 XRF
spectrometer was employed to characterize all synthesized Figure 1. Thermal decomposition behavior of raw-CaCO3 starting
compounds. Table 2 presents the chemical compositions of material derived from scallop shell waste.
scallop-derived CaCO3 and its calcium lactate products.
Calcium oxide (CaO) and oxygen (O) are the major chemical
composition of CaCO3. However, some trace impurities such show the thermal decomposition behavior of scallop-derived
as magnesium (Mg), sulfur (S), phosphorus (P), and CaCO3 sample by presenting the decomposition temperature
potassium (K) were also observed. Four synthesized calcium range of the sample. The TG mass loss and DTG peak were
lactate samples (CaLT-40, CaLT-50, CaLT-60, and CaLT-70) found to have one thermal decomposition period (single step)
mainly contain calcium oxide (69.56−70.88%) and oxygen of about 600−800 °C. Moreover, according to the TG curve,
(26.50−29.30%) contents and minor elemental impurities (S, the remaining calcium lactate mass was 57.97%. A DTG peak
K, P, Mg, and Na). The S and P elements of about <1% may at 843 °C with the DTG value of −0.159 μg·min−1 was
come from calcium sulfate and calcium phosphate, which were assigned to the elimination of a carbon dioxide molecule.
impurities in scallop shells. The presence of SO42− and PO43− It is well known that the products of the thermal
ions may be confirmed by vibrational bands in the Fourier decomposition of CaCO3 are solid-state CaO and gas-state
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Figure 2. Thermal decomposition behaviors of CaCO3-derived calcium lactate products (CaLT-40, CaLT-50, CaLT-60, and CaLT-70) prepared at
different lactic acid concentrations: (a) TG curves and (b) DTG curves.

CO2.3 The compositions of thermodecomposed CaO and CO2 the mass loss with three thermal decomposition steps. The first
products of approximately 57.97 and 43.03 wt % were step is in the range of 100−300 °C. The corresponding DTG
observed, respectively.3 The result indicates clearly that the peak at 89 °C with a DTG peak value of about −0.0148 μg·
hypochlorite treatment in the process of the scallop shell min−1 is assigned as the loss of adsorbed water that existed on
preparation can remove the organic material. Consequently, eq the surface of the synthesized Ca(C2H4OHCOO)2·H2O
1 can be used to present the thermal decomposition of scallop- sample, whereas the DTG peak at 275 °C with DTG peak
derived CaCO3 powder. value of about −0.0087 μg·min−1 is the dehydration process,
resulting in the formation of calcium lactate anhydrous
CaCO3(s) → CaO(s) + CO2 (g) (1)
(Ca(C2H4OHCOO)2). The second step is in the range of
The thermal decompositions of calcium lactate monohydrate 350−500 °C. Its DTG peak at 393 °C with a DTG peak value
products were also investigated. Figure 2a,b, respectively, of about −0.0075 μg·min−1 is the decomposition of Ca-
shows the TG and DTG thermograms of all calcium lactate (C2H4OHCOO)2 to the CaCO3. The final step is in the range
samples (CaLT-40, CaLT-50, CaLT-60, and CaLT-70). The of 600−700 °C. Its DTG peak at 708 °C with a DTG peak
mass loss percentages in the range of 30−1000 °C as shown in value of about −0.0095 μg·min−1 is the decarbonation process,
the TG curves related well to the DTG peaks, indicating the and CaO was thermally formed. The total mass loss to obtain
decomposition mechanism of thermal reactions. Obviously, the the final thermal decomposition product (CaO) was 58.11%.
patterns of the TG and DTG curves of CaLT-40, CaLT-50, The TG and DTG curves of CaLT-50 show similar results to
CaLT-60, and CaLT-70 were similar. Three steps of the mass the CaLT-40. Three thermal decomposition steps were
losses observed in TG curves for all calcium lactates appeared observed. The DTG peaks of the first step (20−250 °C) at
in the range of 100−200, 200−600, and 600−800 °C. Their 118 °C with a DTG peak value of −0.0742 μg·min−1 are
corresponding DTG peaks at about 98−118, 285, 384−393, assigned to the loss of adsorbed water that existed on the
and 688 °C related to the elimination of water H2O surface of Ca(C2H4OHCOO)2·H2O, whereas the DTG peak
(dehydration process), ethyl 2-hydroxypropanoate (C5H10O3 at 285 °C (DTG peak at −0.0663 μg·min−1) is the
or CH3CHOHCOOC2H5), and carbon dioxide CO2 (de- dehydration process to form Ca(C2H4OHCOO)2. The DTG
carbonation process), respectively. The total mass loss was peak of the second step (250−550 °C) at 384 °C (DTG peak
about 58%, which corresponded to the retained mass of about at −0.0471 μg·min −1 ) is the decomposition of Ca-
42%. Therefore, the thermal decomposition mechanism of (C2H4OHCOO)2 to form CaCO3. The DTG peak of the
scallop-derived Ca(C2H4OHCOO)2·H2O resulted in the final step (600−700 °C) at 688 °C (DTG peak at −0.0482 μg·
formation of calcium oxide (CaO), which can be described min−1) is the decarbonation process to form CaO. The total
in the following equations (eqs 2−4). mass loss was 60.16%. Three thermal decomposition steps of
First step: Elimination of H2O (dehydration process) CaLT-60 as shown in the TG and DTG curves were also
observed. The DTG peaks of the first step (100−300 °C) at 99
Ca(C2H4OHCOO)2 · H 2O(s) °C (DTG peak at −0.0324 μg·min−1) are assigned to the loss
→ Ca(C2H4OHCOO)2 (s) + H 2O(g) (2)
of adsorbed water, whereas the DTG peak at 286 °C (DTG
peak at −0.0210 μg·min−1) is the dehydration process. The
Second step: Elimination of ethyl lactate DTG peak of the second step (350−500 °C) at 394 °C (DTG
(CH3CHOHCOOC2H5) peak at −0.0192 μg·min−1) is the decomposition of Ca-
(C2H4OHCOO)2. The DTG peak of the final step (600−700
Ca(C2H4OHCOO)2 (s) °C) at 738 °C (DTG peak at −0.0176 μg·min−1) is the
→ CaCO3(s) + CH3CHOHCOOC2H5(g) (3) decarbonation process. The total mass loss was 57.78%.
According to the TG and DTG curves, CaLT-70 also exhibited
Final step: Elimination of CO2 (decarbonation process) three thermal decomposition steps. The DTG peaks at 99 °C
CaCO3(s) → CaO(s) + CO2 (g) (DTG peak at −0.0246 μg·min−1, first step, 100−300 °C) is
(4)
assigned to the loss of adsorbed water, whereas the DTG peak
The thermal decomposition of each calcium lactate mono- at 286 °C (DTG peak at −0.0134 μg·min−1) is the
hydrate was additionally described in detail. The TG and DTG dehydration process. The DTG peak at 394 °C (DTG peak
curves of the CaLT-40 sample show the temperature range and at −0.0150 μg·min−1, second step, 350−500 °C) is the
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Figure 3. Infrared adsorption spectrum of (a) scallop =0derived CaCO3 and (b) CaCO3-derived calcium lactate products (CaLT-40, CaLT-50,
CaLT-60, and CaLT-70) prepared at different lactic acid concentrations.

Figure 4. X-ray diffraction (XRD) patterns of (a) raw-CaCO3 starting material derived from scallop shell waste and (b) CaCO3-derived calcium
lactate products (CaLT-40, CaLT-50, CaLT-60, and CaLT-70) prepared at different lactic acid concentrations.

decomposition of Ca(C2H4OHCOO)2. The last DTG peak at 2924 cm−1 were the combination and overtone of the
728 °C (DTG peak at −0.0122 μg·min−1, final step, 600−700 symmetric and asymmetric stretching modes of the C−O
°C) is the decarbonation process. The total mass loss was bond, which are the vibrational characteristics of the CO32− of
59.28%. Therefore, based on the results of the TGA technique aragonite polymorph of CaCO3.3,37 The bands in the
as shown in Figure 2, the results confirmed the identity of wavenumber range of 3010−3680 cm−1 are assigned to the
calcium lactate monohydrate (Ca(C2H4OHCOO)2·H2O), vibrational characteristics of both symmetric and asymmetric
which was successfully synthesized by the reaction between stretching modes of C−H of methyl (−CH3) group and O−H
scallop-derived CaCO3 powder and lactic acid at the of water (H2O) that were physically adsorbed on the sample
concentrations of 40, 50, 60, and 70 wt %. surface.
2.4. Infrared Spectroscopy. A PerkinElmer Spectrum GX Figure 3b presents the infrared adsorption spectra of
FTIR spectrophotometer was used to investigate the vibra- CaCO3-derived calcium lactate products (CaLT-40, CaLT-
tional characteristics of scallop-derived CaCO3 (precursor) 50, CaLT-60, and CaLT-70) prepared at different lactic acid
and its calcium lactate products (CaLT-40, CaLT-50, CaLT- concentrations. Obviously, the obtained infrared spectra are
60, and CaLT-70). Figure 3 presents the infrared adsorption similar for all calcium lactates. The broad bands of the infrared
results of the precursor and calcium lactates prepared by adsorption region of about 3030−3740 cm−1 were assigned to
various lactic acid concentrations (40, 50, 60, and 70 wt %). the O−H stretching mode of H2O (in both symmetric and
The adsorption spectrum of the CaCO3 precursor as shown in asymmetric modes) in the crystal structure of Ca-
Figure 3a indicates the vibrational characteristic of carbonate (C2H4OHCOO)2·H2O. The adsorption peaks at about 1746,
(CO32−) anion that is presented in the crystal structure of 1573, and 1487 cm−1 were attributed to the stretching mode of
CaCO3.34−36 Some dominating adsorption peaks were the carbonyl CO group. As described by Pavia et al.,38 the
explained in detail. An absorption peak at about 1440 cm−1 vibrational mode of the CO bond was observed at the
was assigned to the asymmetric stretching mode of the C−O adsorption wavenumber range of 1850−1650 cm−1. In
bond, which is the major adsorption characteristic of CO32−. addition, the results observed in this research are in line with
An infrared peak at about 1801 cm−1 is described as the the results reported by Lee and Kim39 and Cheong.40 Lee and
vibrational stretching mode of the carbonyl CO group. A Kim prepared calcium lactate using black snail (Semisulcospira
vibrational position at about 875 cm−1 is the symmetric libertina (bensoni)) as the CaCO3 precursor, and the obtained
stretching mode of the C−O bond, whereas a vibrational black-snail-derived calcium lactate was then characterized by
position at about 712 cm−1 is the out-of-plane and in-plane the infrared adsorption technique.39 They reported that the
bending of CO32−. Two vibrational bands at about 2523 and peaks at 1592 and 1430 cm−1 were assigned to the asymmetric
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and symmetric stretching modes of the carboxylate RCOO−

functional group. The weak adsorption bands at about 3030−
2852 cm−1 and about 1515−1340 cm−1 were assigned to the
stretching and bending modes of the C−H bond. The
adsorption bands at about 1131−1000 and 670−600 cm−1
could be assigned to ν3 and ν4 modes of the SO42− and/or
PO43−anions, which are observed in the same regions.36 This
result is consistent with the presence of S and P elemental
impurities in the XRF results
2.5. X-ray Diffraction. An X-ray diffractometer with the
Cu Kα X-ray light source was used to investigate and confirm
the crystal structure of the samples prepared in this research. Figure 5. Scanning electron microscopy (SEM) image of raw-CaCO3
The diffraction pattern of the synthesized compound that was starting material derived from scallop shell waste.
prepared from the scallop shell is shown in Figure 4a, pointing
out the diffraction characteristics of calcium carbonate
(CaCO3). The obtained diffraction patterns of CaCO3 powder The calcium lactate monohydrates synthesized from the shell-
exhibit the calcite polymorph according to the PDF #47-1743 derived CaCO3 material and 40 (Figure 6a) or 50 (Figure 6b)
database.41 The diffraction positions (2θ) at 23.01, 29.34, wt % lactic acid were found to be similar. They were thin,
31.35, 35.93, 39.44, 43.16, 47.07, 47.42, 48.44, 56.49, 56.62, overlapping, and shapeless sheets (about 50 μm in size). On
57.32, and 57.47° are the characteristic of calcite CaCO3 the other hand, when 60 wt % lactic acid was used as the
structure.3,42 In addition, the 2θ value at 29.34 corresponded reagent to prepare calcium lactate monohydrate, the irregularly
to the hkl plane of 104, which is the main characteristic of agglomerated hexagonal rods (approximately 50 μm in size)
calcite CaCO3 polymorph with a trigonal crystal system.43 The shown in Figure 6c were observed. In the case of 70 wt % lactic
space group of calcite CaCO3 are R3̅c. The lattice parameters acid, the rectangular shape shown in Figure 6d is arranged in
are a = 4.97630 Å and c = 17.0904 Å, whereas the lattice an orderly manner. These rectangular crystals did not clump
volume is 366.520 Å3.44 The bond lengths between Ca−O and together and were approximately 30 μm in size.
C−O are 2.3574 and 1.2836 Å, respectively.45 Figure 4b shows
the diffraction pattern of CaCO3-derived calcium lactate 3. CONCLUSIONS
products (CaLT-40, CaLT-50, CaLT-60, and CaLT-70) Calcium lactate, which can be applied in various applications,
prepared at different lactic acid concentrations. The pattern was successfully synthesized from the reaction between scallop-
results of all obtained products were compared with those of derived calcite CaCO3 precursor and various lactic acid
calcium lactate reported in the literature,19,46,47 which concentrations (40, 50, 60, and 70 wt %). This work presented
exhibited the diffraction characteristics of calcium lactate some valuable information for the calcium lactate production
(Ca(C2H4OHCOO)2·H2O). The XRD patterns of CaLT-50, using biowaste as starting material. This shell-derived CaCO3
CaLT-60, and CaLT-70 samples are quite similar, which are preparation can be beneficially used to replace the usages of
slightly different from those of CaLT-40, observed at around natural lime or dolomite ores obtained from non-living things
11°. This indicates that the amorphous phase of calcium which are limited resources. Through an experimental design,
acetate monohydrate of a CaLT-40 is different from solid the efficiency of the preparation of calcium lactate was studied
phases of other samples.46,47 All obtained patterns of CaLT by considering the effect of lactic acid concentration on the
samples are in good agreement with the reference data19,46,48 reaction temperature, time consumption, and production yield
and agree with observations from IR and TGA. observed from the calcium lactate production. It was found
2.6. Morphology. LEO VP1450 SEM was used to that the reaction temperature increased with increasing lactic
investigate the morphological characteristics of the prepared acid concentration, and 70 wt % of lactic acid is the suitable
CaCO3 starting material derived from scallop shell waste and concentration to use in the calcium lactate preparation. The
the CaCO3-derived calcium lactate products (CaLT-40, CaLT- single and triple steps were observed from the thermal
50, CaLT-60, and CaLT-70) prepared at different lactic acid decomposition of scallop-derived CaCO3 and its calcium
concentrations. The results of the morphological identity at a lactate products, respectively, and CaO was the final thermal
magnification of 20,000 times showed that the SEM image of decomposition product. All applying characterization techni-
the scallop-derived CaCO3 as shown in Figure 5 had a prism- ques confirmed that the reaction product obtained from
like structure, together with islands (about 5 μm in size), which scallop shell powders was calcium lactate monohydrate
were probably a result of the broken shell. (Ca(C2H4OHCOO)2·H2O). The infrared adsorption and X-
From the previous research, calcium lactate was used in the ray diffraction results of the synthesized calcium lactates are
pharmaceutical application as a calcium source for preventing well consistent with those of previous reports. The
and treating calcium deficiencies because of its good solubility morphologies of the calcium lactates observed from the
and bioavailability.19 Therefore, the morphology and crystal electron microscope exhibited differences in both shapes and
size of the synthesized calcium lactate product were also sizes, which depended on the lactic acid concentrations.
characterized because the morphology and crystal size of the
product may influence its performance after applying in the 4. EXPERIMENTAL SECTION
pharmaceutical field. The morphological identity at 2000 times 4.1. Raw Material Preparations. Scallop shell waste (20
magnification shown in Figure 6 revealed that calcium lactate kg) was collected from a shell dumping place in Bangpoo
monohydrate in four samples obtained from CaCO3 reacted district (location: 13.517 457 591 626 444,
with lactic acid differed in both shape and size according to the 100.654 937 526 486 28), Samut Prakarn province, Thailand;
concentrations of the reacting acid (40, 50, 60, and 70 wt %). 14% sodium hypochlorite aqueous solution (density: 1.21 g·
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Figure 6. Scanning electron microscopy (SEM) images of CaCO3-derived calcium lactate products ((a) CaLT-40, (b) CaLT-50, (c) CaLT-60, and
(d) CaLT-70) prepared at different lactic acid concentrations.

mL−1) was used to clean the scallop waste, and the cleaning the synthesis of calcium lactate products. Each beaker
process was finished when the meat and dust particles of the contained 10 g of scallop-derived CaCO3 powder. The first
scallop were removed completely. The cleaned waste was dried beaker was immediately added with 37 mL of 40 wt % lactic
at 100 °C for 1 h using an oven. After that, the cleaned and acid. The mixture was then stirred continuously for 5 min
dried waste was ground to obtain scallop-derived CaCO3 using a stirring grass rod. The mixing reaction was an
powders and then sieved with 100 meshes, obtaining exothermic process, whereas carbon dioxide (CO2) (reacted
approximately 140 μm of powder particle size. Using this product) and water (reaction medium) were released and
preparing process, the cost of scallop-derived CaCO3 powders evaporated simultaneously. Using this preparation technique,
is no more than 0.03 USD per kg. The prepared CaCO3 calcium lactate was formed. The obtained mixture was then
powder was then used as a low-cost starting material for exposed to ambient conditions (air environment and 1 atm)
calcium lactate synthesis. without applying any other temperature for about 3 h to dry
Industrial-grade lactic acid (88 wt % C2H4OHCOOH, itself, and the completely dried powder was obtained. The
concentrated solution) was also employed without further synthesized calcium lactate product using 40 wt % lactic acid
purification as another starting reagent to synthesize the was designated and labeled as CaLT-40. For the other three
calcium lactate. This concentrated acid was first diluted with beakers, the processes were repeated by replacing 40 wt %
distilled water to prepare four different concentrations of lactic lactic acid by 50, 60, and 70 wt % lactic acids using the acid
acids (40, 50, 60, and 70 wt %). It is well known that the volumes of 30, 25, and 22 mL, respectively. The completely
strongly exothermic process was observed during the dilution dried powders were obtained at the exposure time of about 2 h,
procedure. Therefore, before further use, the diluted acid 45, and 30 min, and the products were labeled as CaLT-50,
solutions were left to cool down. The prices of 40, 50, 60, and CaLT-60, and CaLT-70, respectively. The production yield of
70 wt % lactic acid solutions were calculated and found to be calcium lactate according to eq 5 was calculated using eq 6
approximately 2.07, 2.58, 3.10, and 3.62 USD·kg−1, respec- mobs
tively. yield(%) = × 100
4.2. Calcium Lactate Production. The target com- mtheor (6)
pounds, calcium lactate Ca(C2H4OHCOO)2·nH2O with
different physicochemical compositions and properties, were where mobs and mtheor are the mass of the obtained calcium
synthesized based on the following chemical reaction as shown lactate powder in the preparation process from each lactic acid
in eq 5 concentration and the mass of the theoretical calcium lactate
product, respectively.
CaCO3(s) + 2C2H4OHCOOH(aq) 4.3. Characterization. Chemical contents and impurities
of starting material (scallop waste-derived CaCO3) and four
→ Ca(C2H4OHCOO)2 ·nH 2O(s) + CO2 (g) (5) synthesized calcium lactate (CaLT-40, CaLT-50, CaLT-60,
and CaLT-70) samples were characterized and identified by an
The synthesis method of calcium lactate was described as SRS 3400 X-ray fluorescence spectrometer (XRF, Bruker). The
follows. Four beakers for each lactic acid concentration (40, 50, crystal structure and the purity of the synthesized compounds
60, and 70 wt %) were used to mix the starting reactants for were identified by an X-ray powder diffractometer (XRD;
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Bruker AXS) with the Cu Kα spectral line (λ = 1.54056 Å) as King Mongkut’s Institute of Technology Ladkrabang,
the incident radiation. The resulting XRD patterns were Bangkok 10520, Thailand
compared to the Powder Diffraction File (PDF) database49 Wimonmat Boonmee − Department of Biology, School of
created by the International Centre for Diffraction Data Science, King Mongkut’s Institute of Technology Ladkrabang,
(ICDD) for the identification of the compounds synthesized in Bangkok 10520, Thailand
this research. The 2θ angles, ranged from 10 ot 60° for CaCO3 Complete contact information is available at:
and from 5 to 60° for calcium lactate, were measured with a https://pubs.acs.org/10.1021/acsomega.2c00112
scan speed of 1 s per step at a 0.01° increment to increase the
reliability of the experimental data.50 Infrared adsorption Notes
spectra were recorded by a Spectrum GX Fourier transform
infrared spectrophotometer (FTIR, PerkinElmer) from 4000 The authors declare no competing financial interest.
to 400 cm−1 with 16 scans at a resolution of 4 cm−1. To
prepare the sample for infrared adsorption rest, 1 mg of each
sample was homogeneously mixed with 10 mg of potassium
■ ACKNOWLEDGMENTS
This work was supported by the Thailand Science Research
bromide (KBr, spectroscopic grade) powder.50 A Pyris and Innovation (TSRI) (RE-KRIS/008/64). The authors
Diamond thermogravimetric analyzer (TGA, PerkinElmer) thank the Scientific Instruments Center KMITL for supporting
was implemented to investigate the thermal decomposition TGA, FTIR, XRD, and SEM techniques.

■
behavior of the sample. Thermogravimetric (TG) and
differential thermogravimetric (DTG) curves of samples were
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