CN108217709A - A kind of method that calcium chloride is prepared in the production process using chitin - Google Patents
A kind of method that calcium chloride is prepared in the production process using chitin Download PDFInfo
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- CN108217709A CN108217709A CN201611153325.9A CN201611153325A CN108217709A CN 108217709 A CN108217709 A CN 108217709A CN 201611153325 A CN201611153325 A CN 201611153325A CN 108217709 A CN108217709 A CN 108217709A
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- calcium chloride
- hydrochloric acid
- pickle liquor
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- production process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods that calcium chloride is prepared in production process using chitin, include the following steps：5%~6% hydrochloric acid solution is taken to impregnate shrimp and crab shells to carry out impregnating reaction for the first time, concentration of hydrochloric acid is reduced to 0.4 0.5% for the first time, and the Baume degrees of calcium chloride rises to Be °, obtains the first pickle liquor；It adjusts concentration of hydrochloric acid in the first pickle liquor to carry out impregnating reaction for the second time to 5%~6%, concentration of hydrochloric acid is reduced to 0.4 0.5% for the second time, 9~10Be ° of calcium chloride solution Baume degrees；It repeats the above steps 7~8 times and carries out final immersion reaction, concentration of hydrochloric acid is reduced to 0.5%, and 32~35Be ° of calcium chloride solution Baume degrees obtains final pickle liquor；Lime or lime stone is taken to carry out neutralization reaction with final pickle liquor；Decoloration removal of impurities；Condensing crystallizing；Dry, crush, being sieved, packing and to obtain calcium chloride.The preparation method reduces sewage discharge, increases economic benefit, is prepared into food-grade calcium chloride.
Description
Technical field
The invention belongs to Calcium Chloride Production technical field, a kind of more particularly to utilize in chitin production process prepares chlorination
The method of calcium.
Background technology
It is dense with mass percent in chitin production process (traditional handicraft) containing calcium salt 30% or so in shrimp and crab shells
The hydrochloric acid solution of degree 5%~6% impregnates reaction, forms the calcium chloride solution containing other organic impurities, usually after environmental protection treatment,
Directly externally discharge, increases quantity of wastewater effluent, not only brings load to environment, but also increase the cost of manufacturing enterprise.Cause
How this reduces entreprise cost, and reducing environmental pollution has become the main problem that chitin manufacturing enterprise faces.
Invention content
In view of the above-mentioned problems of the prior art, it is an object of the invention to provide a kind of using in chitin production process
The method for preparing calcium chloride reduces the sewage discharge in chitin production, increases economic benefit.
The purpose of the present invention will be achieved by the following technical programs：
A kind of method that calcium chloride is prepared in production process using chitin, includes the following steps：1) mass percent is taken
5%~6% hydrochloric acid solution of concentration impregnates shrimp crab, carries out impregnating reaction for the first time, hydrochloric acid mass percent concentration is reduced to for the first time
0.4-0.5%, calcium chloride solution obtain Baume degrees and rise to 4-5Be °, obtain the first pickle liquor；
2) it adds in concentrated hydrochloric acid to the first pickle liquor, hydrochloric acid mass percent concentration is made to reach 5%~6% again, carry out
Second impregnates reaction, and hydrochloric acid mass percent concentration is reduced to 0.4-0.5% for the second time, and calcium chloride solution Baume degrees rises to 9~
10Be °, obtain the second pickle liquor；
3) 7~8 times are recycled according to this to when carrying out final immersion reaction, hydrochloric acid mass percent concentration is finally reduced to 0.5%,
Calcium chloride solution Baume degrees rises to 32~35Be °, obtains final pickle liquor；
4) lime or lime stone is taken to carry out neutralization reaction with final pickle liquor, pH value reaches 7.0-7.5, obtains neutralization reaction
Liquid；
5) the neutralization reaction liquid described in step 4) is subjected to decoloration removal of impurities, press filtration must clarify destainer；
6) by the destainer condensing crystallizing described in step 5), the calcium chloride containing two crystallizations water is obtained；
7) it by 120 DEG C of the calcium chloride drying two hours containing two crystallizations water described in step 6), crushes, sieving, pack,
Up to calcium chloride.
The method that calcium chloride is prepared in a kind of above-mentioned production process using chitin, the matter of concentrated hydrochloric acid described in step 2)
It is 30% to measure percent concentration.
The method that calcium chloride is prepared in a kind of above-mentioned production process using chitin, the decoloration removal of impurities described in step 5)
Include the following steps：In neutralization reaction liquid respectively plus described in food grade active charcoal, EDTA to step 4), 60 DEG C of stirring decolorations 30
Minute, plate compression must clarify destainer.
The method that calcium chloride is prepared in a kind of above-mentioned production process using chitin, the food grade active charcoal with it is described
The volume ratio of neutralization reaction liquid is 0.3ml: 100ml.
The method that calcium chloride is prepared in a kind of above-mentioned production process using chitin, condensing crystallizing specifically walks in step 6)
Suddenly it is：The destainer is concentrated in vacuo to 55Be ° of Baume degrees or more, crystallisation by cooling 4 hours is then centrifuged for detaching, obtains band
The calcium chloride of two crystallizations water.
Compared with prior art, the side of calcium chloride is prepared in a kind of production process using chitin provided by the present invention
Method has reached following technique effect：Compared to traditional handicraft, the sewage discharge in chitin production, environment friend are greatly reduced
It is good, increase the economic benefit of chitin production, improve profit, the product calcium chloride of preparation is food-grade calcium chloride.
Below just in conjunction with the embodiments, the embodiment of the present invention is described in further detail, so that the technology of the present invention
Scheme is more readily understood, grasps.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.In following embodiments
The experimental method is conventional method unless otherwise specified；The reagent and material, unless otherwise specified, can be from business
Approach obtains.
Embodiment one
1) 5% hydrochloric acid solution 50ml of mass percent concentration is taken to impregnate shrimp crab 35g, carries out impregnating reaction for the first time, treats salt
Sour mass percent concentration is reduced to 0.4% for the first time, and calcium chloride solution Baume degrees rises to 4Be °, obtains the first pickle liquor 50ml；
2) it adds in 6.5ml 30% concentrated hydrochloric acids to the first pickle liquor, hydrochloric acid mass percent concentration is made to reach 5% again,
It carries out second and impregnates reaction, treat that hydrochloric acid mass percent concentration is reduced to 0.4% again, calcium chloride solution Baume degrees rises to
9Be °, obtain the second pickle liquor 50ml；
3) it recycles 7 times according to this, final to impregnate reaction, final soak hydrochloric acid mass percent concentration is reduced to 0.4%, chlorination
Calcium solution Baume degrees rises to 32Be °, obtains final pickle liquor 50ml；
Wherein, also containing the impurity such as a considerable amount of chromoproteins in final pickle liquor, pickle liquor in recycling not
Influence chitin product quality.
4) neutralization reaction is carried out with the final pickle liquor 50ml described in lime stone 10g and step 3), pH value reaches 7.0, obtains
Neutralization reaction liquid 55ml；
Wherein the reaction principle of the step is CaCO3+2HCL→CaCL2+H2O+CO2↑；
5) decoloration removal of impurities：Add the food grade active charcoal (body of food grade active charcoal and the neutralization reaction liquid of 0.3% quantity
Product is than for 0.3ml: 100ml) and EDTA 0.2g to neutralization reaction liquid in, 60 DEG C of stirring decolorations 30 minutes, plate compression obtains clear
Clear destainer 55ml；
6) condensing crystallizing：Above-mentioned destainer -0.85mpa, 70 DEG C are concentrated in vacuo to 55Be ° of solution Baume degrees or more, are opened
Cooling water is opened, crystallisation by cooling 4 hours is then centrifuged for detaching, and obtains the calcium chloride 14.8g containing two crystallizations water；
7) above-mentioned 120 DEG C of the calcium chloride drying two hours containing two crystallizations water is crushed, sieving, is packed to get calcium chloride
11g。
It is food-grade calcium chloride using calcium chloride made from the method for the present embodiment.
Embodiment two
1) 6% hydrochloric acid solution 50ml of mass percent concentration is taken to impregnate shrimp crab 35g, carries out impregnating reaction for the first time, treats salt
Sour mass percent concentration is reduced to 0.5% for the first time, and calcium chloride solution Baume degrees rises to 5Be °, obtains the first pickle liquor 50ml；
2) it adds in 6.4ml30% concentrated hydrochloric acids to the first pickle liquor, hydrochloric acid mass percent concentration is made to reach 6% again,
It carries out second and impregnates reaction, treat that hydrochloric acid mass percent concentration is reduced to 0.5% again, calcium chloride solution Baume degrees rises to
10Be °, obtain the second pickle liquor 50ml；
3) it recycling 7 times according to this, carries out final impregnate and react, final soak hydrochloric acid mass percent concentration is reduced to 0.5%,
35Be ° of calcium chloride solution Baume degrees obtains final pickle liquor 52ml；
Wherein, also containing impurity such as a considerable amount of chromoproteins in final pickle liquor, pickle liquor is recycling not shadow
Ring chitin product quality.
4) neutralization reaction is carried out with the final pickle liquor 50ml described in lime 10.5g and step 3), pH value reaches 7.5, obtains
Neutralization reaction liquid 55ml；
Wherein the reaction principle of the step is CaO+2HCL → CaCL2+H2O
5) decoloration removal of impurities：Add the food grade active charcoal (body of food grade active charcoal and the neutralization reaction liquid of 0.3% quantity
Product is than for 0.3ml: 100ml) and EDTA0.2g to neutralization reaction liquid in, 60 DEG C of stirring decolorations 30 minutes, plate compression must be clarified
Destainer 55ml；
6) condensing crystallizing：Above-mentioned destainer -0.85mpa, 70 DEG C are concentrated in vacuo to 55Be ° of solution Baume degrees or more, are opened
Cooling water is opened, crystallisation by cooling 4 hours is then centrifuged for detaching, and obtains the calcium chloride 15g containing two crystallizations water；
7) 120 DEG C of the calcium chloride drying two hours containing two crystallizations water described in is crushed, sieving, is packed to get calcium chloride
11.5g。
It is food-grade calcium chloride using calcium chloride made from the method for the present embodiment.
Embodiment three
1) 5.5% hydrochloric acid solution 50ml of mass percent concentration is taken to impregnate shrimp crab 35g, carries out impregnating reaction for the first time, treat
Hydrochloric acid mass percent concentration is reduced to 0.45% for the first time, and calcium chloride solution Baume degrees rises to 4.5Be °, obtains the first pickle liquor
50ml；
2) it adds in 6.3ml30% concentrated hydrochloric acids to the first pickle liquor, hydrochloric acid mass percent concentration is made to reach again
5.5%, it carries out second and impregnates reaction, treat that hydrochloric acid mass percent concentration is reduced to 0.5% again, calcium chloride solution Baume degrees liter
To 9.5Be °, the second pickle liquor 50ml is obtained；
3) aforesaid operations are repeated 8 times, carries out final impregnate and react, final soak residual hydrochloric acid mass percent concentration drop
It is 0.5%, 33Be ° of calcium chloride solution Baume degrees obtains final pickle liquor 50ml；
Wherein, also containing impurity such as chromoproteins in final pickle liquor, pickle liquor recycling does not influence chitin product
Quality.
4) neutralization reaction is carried out with the final pickle liquor 50ml described in lime 10.2g and step 3), pH value reaches 7.2, obtains
Neutralization reaction liquid 55ml；
Wherein the reaction principle of the step is CaO+2HCL → CaCL2+H2O
5) decoloration removal of impurities：Add the food grade active charcoal (body of food grade active charcoal and the neutralization reaction liquid of 0.3% quantity
Product is than for 0.3ml: 100ml) and EDTA0.2g to neutralization reaction liquid in, 60 DEG C of stirring decolorations 30 minutes, plate compression must be clarified
Destainer 55ml；
6) condensing crystallizing：Above-mentioned destainer -0.85mpa, 70 DEG C are concentrated in vacuo to 55Be ° of solution Baume degrees or more, are opened
Cooling water is opened, crystallisation by cooling 4 hours is then centrifuged for detaching, and obtains the calcium chloride 15.5g containing two crystallizations water；
7) 120 DEG C of the calcium chloride drying two hours containing two crystallizations water described in is crushed, sieving, is packed to get calcium chloride
11.8g。
It is food-grade calcium chloride using calcium chloride made from the method for the present embodiment.
The calcium chloride of the example IV present invention be food-grade calcium chloride, embodiment one~tri- prepare food-grade calcium chloride
Test result is shown in Table 1.
1 embodiment of table, one~tri- food-grade calcium chloride testing result
It is learnt by table 1, calcium chloride prepared by 1-3 of the embodiment of the present invention meets food-grade calcium chloride standard.
Several preferred embodiments of the present invention have shown and described in above description, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations,
Modification and environment, and the above teachings or related fields of technology or knowledge can be passed through in the scope of the invention is set forth herein
It is modified.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be in this hair
In the protection domain of bright appended claims.
Claims (5)
1. the method for calcium chloride is prepared in a kind of production process using chitin, which is characterized in that include the following steps：1) matter is taken
It measures percent concentration 5%~6% hydrochloric acid solution and impregnates shrimp crab, carry out impregnating reaction for the first time, hydrochloric acid mass percent concentration the
0.4-0.5% once is reduced to, the Baume degrees of calcium chloride solution rises to 4-5Be °, obtains the first pickle liquor；
2) it adds in concentrated hydrochloric acid to the first pickle liquor, hydrochloric acid mass percent concentration is made to reach 5%~6% again, carry out second
Secondary to impregnate reaction, hydrochloric acid mass percent concentration is reduced to 0.4-0.5% again, and calcium chloride solution Baume degrees rises to 9~10Be °,
Obtain the second pickle liquor；
3) 7~8 times are recycled according to this to when carrying out final immersion reaction, hydrochloric acid mass percent concentration is reduced to 0.4-0.5% again,
Calcium chloride solution Baume degrees rises to 32~35Be °, obtains final pickle liquor；
4) lime or lime stone is taken to carry out neutralization reaction with final pickle liquor, pH value reaches 7.0-7.5, obtains neutralization reaction liquid；
5) the neutralization reaction liquid described in step 4) is subjected to decoloration removal of impurities, press filtration must clarify destainer；
6) by the destainer condensing crystallizing described in step 5), the calcium chloride containing two crystallizations water is obtained；
7) by 120 DEG C of calcium chloride drying two hours containing two crystallizations water described in step 6), crush, sieving, packaging to get
Calcium chloride.
2. the method for calcium chloride is prepared in a kind of production process using chitin according to claim 1, which is characterized in that
The mass percent concentration of concentrated hydrochloric acid described in step 2) is 30%.
3. the method for calcium chloride is prepared in a kind of production process using chitin according to claim 1, which is characterized in that
Decoloration removal of impurities described in step 5) includes the following steps：Respectively plus the neutralization described in food grade active charcoal, EDTA to step 4)
In reaction solution, 60 DEG C of stirrings are decolourized 30 minutes, and plate compression must clarify destainer.
4. the method for calcium chloride is prepared in a kind of production process using chitin according to claim 3, which is characterized in that
The volume ratio of the food grade active charcoal and the neutralization reaction liquid is 0.3ml: 100ml.
5. the method for calcium chloride is prepared in a kind of production process using chitin according to claim 1, which is characterized in that
In step 6) condensing crystallizing the specific steps are：The destainer is concentrated in vacuo to 55Be ° of Baume degrees or more, crystallisation by cooling 4 is small
When, it is then centrifuged for detaching, obtains the calcium chloride of two crystallizations water of band.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611153325.9A CN108217709A (en) | 2016-12-14 | 2016-12-14 | A kind of method that calcium chloride is prepared in the production process using chitin |
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| CN201611153325.9A CN108217709A (en) | 2016-12-14 | 2016-12-14 | A kind of method that calcium chloride is prepared in the production process using chitin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110902709A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing calcium chloride by utilizing fluidized bed fly ash |
| CN110903104A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing foamed ceramic and co-producing calcium chloride and polyaluminium chloride by fluidized bed fly ash |
-
2016
- 2016-12-14 CN CN201611153325.9A patent/CN108217709A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110902709A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing calcium chloride by utilizing fluidized bed fly ash |
| CN110903104A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing foamed ceramic and co-producing calcium chloride and polyaluminium chloride by fluidized bed fly ash |
| CN110902709B (en) * | 2018-09-17 | 2021-05-14 | 中国科学院过程工程研究所 | Method for preparing calcium chloride by utilizing fluidized bed fly ash |
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