CN113480424A - Method for producing calcium formate based on sugar mill filter mud - Google Patents
Method for producing calcium formate based on sugar mill filter mud Download PDFInfo
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- CN113480424A CN113480424A CN202110676546.9A CN202110676546A CN113480424A CN 113480424 A CN113480424 A CN 113480424A CN 202110676546 A CN202110676546 A CN 202110676546A CN 113480424 A CN113480424 A CN 113480424A
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- China
- Prior art keywords
- filter mud
- calcium carbonate
- solution
- formic acid
- calcium formate
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 229940044172 calcium formate Drugs 0.000 title claims abstract description 35
- 235000019255 calcium formate Nutrition 0.000 title claims abstract description 35
- 239000004281 calcium formate Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 120
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 60
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 41
- 235000019253 formic acid Nutrition 0.000 claims abstract description 41
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 34
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 34
- 239000004571 lime Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 235000013336 milk Nutrition 0.000 claims abstract description 29
- 239000008267 milk Substances 0.000 claims abstract description 29
- 210000004080 milk Anatomy 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000007865 diluting Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000012452 mother liquor Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000010802 sludge Substances 0.000 claims 5
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention relates to the technical field of industrial production, in particular to a method for producing calcium formate based on sugar mill filter mud, which comprises the following steps: the method comprises the steps of crushing and finely grinding calcium carbonate filter mud, diluting a formic acid solution, diluting a lime milk solution, adding the formic acid solution into the crushed calcium carbonate filter mud, stirring, adding the lime milk solution, controlling and adjusting the pH value of the whole solution to be 6-7, finally performing centrifugal separation treatment on the obtained product, performing air flow drying treatment to obtain a calcium formate product, and continuously recycling mother liquor. According to the method, a large amount of waste filter mud generated in sugar manufacturing can be effectively consumed, the pressure of enterprises on filter mud treatment is reduced, the discharge amount is reduced, the environment is effectively protected, and the calcium formate can be effectively produced on the premise of low cost, low energy consumption and small investment, so that the economic benefit and the social benefit are further improved.
Description
Technical Field
The invention relates to the technical field of industrial production, in particular to a method for producing calcium formate based on sugar mill filter mud.
Background
Refined sugar is a food raw material, and during the production of the refined sugar, a large amount of sugar filter mud is produced, and the sugar filter mud is CaCO produced in the sugar manufacturing process of a sugar factory3About 1 ton of filter mud is discharged per 1 ton of sugar produced as a main component waste, and the sugar filter mud is one of the large byproducts of the sugar industry and is directly used for fertilizing fields or discarded for a long time. The piled filter mud occupies a large amount of soil, and is easy to mildew and smell, breed flies, pollute air and influence sanitation due to the fact that the filter mud contains various organic matters and saccharides.
Most methods for recycling sugar filter mud in the current market are manufacturing industrial raw material lime, producing biological fertilizer and the like, and when the industrial raw material lime is produced, high temperature is needed for calcination for more than 2 hours, so that a large amount of energy is wasted, the production cost is high, and the method is not beneficial to environmental protection; when the biological fertilizer is produced, the water content and the organic nutrient of the filter mud cannot reach the indexes of the biological fertilizer, so that the consumption of the filter mud is limited, and when the calcium formate is produced by a neutralization method, a finished calcium carbonate raw material is required to be used, so that the production cost is increased.
Disclosure of Invention
The invention aims to provide a method for producing calcium formate based on sugar mill filter mud, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for producing calcium formate based on sugar mill filter mud comprises the following steps:
the method comprises the following steps: preparing raw materials: firstly, preparing calcium carbonate filter mud, formic acid solution and lime milk solution, firstly pretreating the calcium carbonate filter mud to remove impurities in the calcium carbonate filter mud, then crushing and grinding the calcium carbonate filter mud, then diluting the formic acid solution to ensure that the purity of the diluted formic acid solution is 60-80%, then diluting the lime milk solution to ensure that the purity of the diluted lime milk solution is 20-30%, and then collecting the raw materials for later use;
step two: and (3) neutralization reaction: adding the diluted formic acid solution in the step one into the crushed calcium carbonate filter mud, then stirring, stirring by adopting equipment of a transverse stirrer during stirring, adding the lime milk solution prepared in the step one after no bubbles are generated, continuing stirring for reaction, controlling and adjusting the pH value of the whole solution to be 6-7 during adding the lime milk solution, and collecting the solution for later use;
step three: extracting calcium formate: and finally, performing centrifugal separation on the product obtained in the step two, and then performing airflow drying treatment to obtain a calcium formate product, wherein the mother liquor is continuously recycled.
Preferably, in the first step, when the calcium carbonate filter mud is subjected to crushing and fine grinding treatment, the particle fineness of the calcium carbonate filter mud is 200-500 meshes.
Preferably, in the second step, the stirring speed is 60r/min, and the stirring is performed until no bubbles are generated.
Preferably, the weight parts of the calcium carbonate filter mud and the formic acid in the second step are 100 parts by weight of the calcium carbonate filter mud and 101 parts by weight of the formic acid.
Preferably, in the second step, when the lime milk solution is added, the solution is placed in a water bath kettle at 80 ℃ for heating.
Preferably, the time of centrifugal dehydration in the third step is 20min, so that the water content of the wet material is less than or equal to 10%, and then a tubular airflow dryer is adopted, and the drying temperature is 150 ℃.
Compared with the prior art, the invention has the beneficial effects that:
according to the method, a large amount of waste filter mud generated in sugar manufacturing can be effectively consumed, the pressure of enterprises on filter mud treatment is reduced, the discharge amount is reduced, the environment is effectively protected, and the calcium formate can be effectively produced on the premise of low cost, low energy consumption and small investment, so that the economic benefit and the social benefit are further improved.
Detailed Description
Example 1: the invention provides a technical scheme that:
a method for producing calcium formate based on sugar mill filter mud comprises the following steps:
the method comprises the following steps: preparing raw materials: firstly, preparing calcium carbonate filter mud, formic acid solution and lime milk solution, firstly pretreating the calcium carbonate filter mud to remove impurities in the calcium carbonate filter mud, then crushing and grinding the calcium carbonate filter mud, then diluting the formic acid solution to ensure that the purity of the diluted formic acid solution is 80%, then diluting the lime milk solution to ensure that the purity of the diluted lime milk solution is 30%, and then collecting the raw materials for later use;
step two: and (3) neutralization reaction: adding the diluted formic acid solution in the step one into the crushed calcium carbonate filter mud, then stirring, stirring by adopting equipment of a transverse stirrer during stirring, adding the lime milk solution prepared in the step one after no bubbles are generated, continuing stirring for reaction, controlling and adjusting the pH value of the whole solution to 7 when adding the lime milk solution, and collecting the solution for later use;
step three: extracting calcium formate: and finally, performing centrifugal separation on the product obtained in the step two, and then performing airflow drying treatment to obtain a calcium formate product, wherein the mother liquor is continuously recycled.
According to the method, a large amount of waste filter mud generated in sugar manufacturing can be effectively consumed, the pressure of enterprises on filter mud treatment is reduced, the discharge amount is reduced, the environment is effectively protected, and the calcium formate can be effectively produced on the premise of low cost, low energy consumption and small investment, so that the economic benefit and the social benefit are further improved.
The particle fineness of the calcium carbonate filter mud is 200 meshes when the calcium carbonate filter mud is crushed and finely ground in the first step, the calcium carbonate filter mud and formic acid solution can have sufficient contact area by the arrangement, so that reaction is convenient to carry out, the stirring speed is 60r/min when stirring in the second step until no bubbles are generated, the arrangement can ensure that the formic acid and the calcium carbonate in the second step can carry out better reaction, so that subsequent production work can be conveniently carried out, the weight ratio of the calcium carbonate filter mud to the formic acid in the second step is 100 parts by weight of the calcium carbonate filter mud and 101 parts by weight of the formic acid, the arrangement can ensure that the formic acid and the calcium carbonate in the calcium carbonate filter mud can fully react, so that better reaction effect is ensured, when the lime emulsion solution is added in the second step, the solution is placed in a water bath kettle at 80 ℃ for heating, the setting can accelerate the adjustment of the pH value and is convenient for subsequent drying treatment, the time of centrifugal dehydration in the third step is 20min, so that the water content of the wet material is less than or equal to 10%, then a tubular airflow dryer is adopted, the drying temperature is 150 ℃, and the setting ensures that the calcium formate is well produced.
Example 2: the invention provides a technical scheme that:
a method for producing calcium formate based on sugar mill filter mud comprises the following steps:
the method comprises the following steps: preparing raw materials: firstly, preparing calcium carbonate filter mud, formic acid solution and lime milk solution, firstly pretreating the calcium carbonate filter mud to remove impurities in the calcium carbonate filter mud, then crushing and grinding the calcium carbonate filter mud, then diluting the formic acid solution to ensure that the purity of the diluted formic acid solution is 70%, then diluting the lime milk solution to ensure that the purity of the diluted lime milk solution is 25%, and then collecting the raw materials for later use;
step two: and (3) neutralization reaction: adding the diluted formic acid solution in the step one into the crushed calcium carbonate filter mud, then stirring, stirring by adopting equipment of a transverse stirrer during stirring, adding the lime milk solution prepared in the step one after no bubbles are generated, continuing stirring for reaction, controlling and adjusting the pH value of the whole solution to 7 when adding the lime milk solution, and collecting the solution for later use;
step three: extracting calcium formate: and finally, performing centrifugal separation on the product obtained in the step two, and then performing airflow drying treatment to obtain a calcium formate product, wherein the mother liquor is continuously recycled.
According to the method, a large amount of waste filter mud generated in sugar manufacturing can be effectively consumed, the pressure of enterprises on filter mud treatment is reduced, the discharge amount is reduced, the environment is effectively protected, and the calcium formate can be effectively produced on the premise of low cost, low energy consumption and small investment, so that the economic benefit and the social benefit are further improved.
The particle fineness of the calcium carbonate filter mud is 350 meshes when the calcium carbonate filter mud is crushed and finely ground in the first step, the calcium carbonate filter mud and formic acid solution can have sufficient contact area by the arrangement, so that reaction is convenient to carry out, the stirring speed is 60r/min when stirring in the second step until no bubbles are generated, the arrangement can ensure that the formic acid and the calcium carbonate in the second step can carry out better reaction, so that subsequent production work can be conveniently carried out, the weight ratio of the calcium carbonate filter mud to the formic acid in the second step is 100 parts by weight of the calcium carbonate filter mud and 101 parts by weight of the formic acid, the arrangement can ensure that the formic acid and the calcium carbonate in the calcium carbonate filter mud can fully react, so that better reaction effect is ensured, when the lime emulsion solution is added in the second step, the solution is placed in a water bath kettle at 80 ℃ for heating, the setting can accelerate the adjustment of the pH value and is convenient for subsequent drying treatment, the time of centrifugal dehydration in the third step is 20min, so that the water content of the wet material is less than or equal to 10%, then a tubular airflow dryer is adopted, the drying temperature is 150 ℃, and the setting ensures that the calcium formate is well produced.
Example 3: the invention provides a technical scheme that:
a method for producing calcium formate based on sugar mill filter mud comprises the following steps:
the method comprises the following steps: preparing raw materials: firstly, preparing calcium carbonate filter mud, formic acid solution and lime milk solution, firstly pretreating the calcium carbonate filter mud to remove impurities in the calcium carbonate filter mud, then crushing and grinding the calcium carbonate filter mud, then diluting the formic acid solution to ensure that the purity of the diluted formic acid solution is 60%, then diluting the lime milk solution to ensure that the purity of the diluted lime milk solution is 20%, and then collecting the raw materials for later use;
step two: and (3) neutralization reaction: adding the diluted formic acid solution in the step one into the crushed calcium carbonate filter mud, then stirring, stirring by adopting equipment of a transverse stirrer during stirring, adding the lime milk solution prepared in the step one after no bubbles are generated, continuing stirring for reaction, controlling and adjusting the pH value of the whole solution to 7 when adding the lime milk solution, and collecting the solution for later use;
step three: extracting calcium formate: and finally, performing centrifugal separation on the product obtained in the step two, and then performing airflow drying treatment to obtain a calcium formate product, wherein the mother liquor is continuously recycled.
According to the method, a large amount of waste filter mud generated in sugar manufacturing can be effectively consumed, the pressure of enterprises on filter mud treatment is reduced, the discharge amount is reduced, the environment is effectively protected, and the calcium formate can be effectively produced on the premise of low cost, low energy consumption and small investment, so that the economic benefit and the social benefit are further improved.
The particle fineness of the calcium carbonate filter mud is 500 meshes when the calcium carbonate filter mud is crushed and finely ground in the first step, the calcium carbonate filter mud and formic acid solution can have sufficient contact area by the arrangement, so that reaction is convenient to carry out, the stirring speed is 60r/min when stirring in the second step until no bubbles are generated, the arrangement can ensure that the formic acid and the calcium carbonate in the second step can carry out better reaction, so that subsequent production work can be conveniently carried out, the weight ratio of the calcium carbonate filter mud to the formic acid in the second step is 100 parts by weight of the calcium carbonate filter mud and 101 parts by weight of the formic acid, the arrangement can ensure that the formic acid and the calcium carbonate in the calcium carbonate filter mud can fully react, so that better reaction effect is ensured, when the lime emulsion solution is added in the second step, the solution is placed in a water bath kettle at 80 ℃ for heating, the setting can accelerate the adjustment of the pH value and is convenient for subsequent drying treatment, the time of centrifugal dehydration in the third step is 20min, so that the water content of the wet material is less than or equal to 10%, then a tubular airflow dryer is adopted, the drying temperature is 150 ℃, and the setting ensures that the calcium formate is well produced.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (6)
1. A method for producing calcium formate based on sugar mill filter mud is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparing raw materials: firstly, preparing calcium carbonate filter mud, formic acid solution and lime milk solution, firstly pretreating the calcium carbonate filter mud to remove impurities in the calcium carbonate filter mud, then crushing and grinding the calcium carbonate filter mud, then diluting the formic acid solution to ensure that the purity of the diluted formic acid solution is 60-80%, then diluting the lime milk solution to ensure that the purity of the diluted lime milk solution is 20-30%, and then collecting the raw materials for later use;
step two: and (3) neutralization reaction: adding the diluted formic acid solution in the step one into the crushed calcium carbonate filter mud, then stirring, stirring by adopting equipment of a transverse stirrer during stirring, adding the lime milk solution prepared in the step one after no bubbles are generated, continuing stirring for reaction, controlling and adjusting the pH value of the whole solution to be 6-7 during adding the lime milk solution, and collecting the solution for later use;
step three: extracting calcium formate: and finally, performing centrifugal separation on the product obtained in the step two, and then performing airflow drying treatment to obtain a calcium formate product, wherein the mother liquor is continuously recycled.
2. The method for producing calcium formate based on sugar mill sludge as claimed in claim 1, wherein the method comprises the following steps: in the first step, when the calcium carbonate filter mud is crushed and ground, the particle fineness of the calcium carbonate filter mud is 200-500 meshes.
3. The method for producing calcium formate based on sugar mill sludge as claimed in claim 1, wherein the method comprises the following steps: and in the second step, stirring is carried out at a speed of 60r/min until no bubbles are generated.
4. The method for producing calcium formate based on sugar mill sludge as claimed in claim 1, wherein the method comprises the following steps: and in the second step, the weight parts of the calcium carbonate filter mud and the formic acid are 100 parts of the calcium carbonate filter mud and 101 parts of the formic acid.
5. The method for producing calcium formate based on sugar mill sludge as claimed in claim 1, wherein the method comprises the following steps: and in the second step, when the lime milk solution is added, the solution is placed in a water bath kettle at the temperature of 80 ℃ for heating.
6. The method for producing calcium formate based on sugar mill sludge as claimed in claim 1, wherein the method comprises the following steps: and in the third step, the time of centrifugal dehydration is 20min, so that the water content of the wet material is less than or equal to 10%, and then a tubular airflow dryer is adopted, and the drying temperature is 150 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110676546.9A CN113480424A (en) | 2021-06-18 | 2021-06-18 | Method for producing calcium formate based on sugar mill filter mud |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110676546.9A CN113480424A (en) | 2021-06-18 | 2021-06-18 | Method for producing calcium formate based on sugar mill filter mud |
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| CN113480424A true CN113480424A (en) | 2021-10-08 |
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| CN202110676546.9A Pending CN113480424A (en) | 2021-06-18 | 2021-06-18 | Method for producing calcium formate based on sugar mill filter mud |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924258A (en) * | 2012-10-31 | 2013-02-13 | 山东中谷淀粉糖有限公司 | Method for producing calcium formate from sugar mill filter mud |
| CN107686446A (en) * | 2017-09-15 | 2018-02-13 | 广汉隆达饲料有限公司 | The preparation method of feed grade calcium formate |
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2021
- 2021-06-18 CN CN202110676546.9A patent/CN113480424A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924258A (en) * | 2012-10-31 | 2013-02-13 | 山东中谷淀粉糖有限公司 | Method for producing calcium formate from sugar mill filter mud |
| CN107686446A (en) * | 2017-09-15 | 2018-02-13 | 广汉隆达饲料有限公司 | The preparation method of feed grade calcium formate |
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