CN111056977A - Preparation method of dicyandiamide - Google Patents
Preparation method of dicyandiamide Download PDFInfo
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- CN111056977A CN111056977A CN201911419286.6A CN201911419286A CN111056977A CN 111056977 A CN111056977 A CN 111056977A CN 201911419286 A CN201911419286 A CN 201911419286A CN 111056977 A CN111056977 A CN 111056977A
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- dicyandiamide
- aqueous solution
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- cyanamide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a preparation method of dicyandiamide, which comprises the following steps: s1, mixing lime nitrogen, water and carbon dioxide, and hydrolyzing and carbonizing to produce cyanamide aqueous solution; s2, heating and polymerizing the cyanamide aqueous solution to produce dicyandiamide aqueous solution; s3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into a dicyandiamide solution, and flocculating and filtering impurities; s4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product. The invention adopts a production process of the composite flocculant taking polyacrylamide and polyethyleneimine as materials, adds the composite flocculant into dicyandiamide solution, performs flocculation precipitation and filtration removal on calcium-containing impurities in the dicyandiamide solution, obviously improves the quality of dicyandiamide, and meets the quality requirement of electronic grade dicyandiamide.
Description
Technical Field
The invention relates to a preparation method of dicyandiamide.
Background
Dicyandiamide (dicyandiamide), abbreviated DICY or DCD. Is a dimer of cyanamide and is also a cyano derivative of guanidine. The chemical formula C2H4N 4. White crystalline powder. Soluble in water, alcohols, ethylene glycol and dimethylformamide, practically insoluble in ether and benzene, non-flammable and stable when dry.
The traditional dicyandiamide preparation method is to hydrolyze calcium cyanamide to obtain calcium cyanamide hydrogen suspension, remove calcium hydroxide filter residue by vacuum filtration, and introduce carbon dioxide into the filtrate to precipitate calcium in the form of calcium carbonate to obtain cyanamide liquid. Polymerizing under alkaline condition, filtering, cooling, crystallizing, separating and drying to obtain dicyandiamide.
The electronic grade dicyandiamide is mainly used in the high-end electronic industry, can be used as an epoxy resin curing agent, an electronic packaging material and the production of an FR-4 copper-clad plate, can also be used as a high-grade coating with higher requirement on the purity of dicyandiamide, an intermediate raw material for chemical pharmacy and the like, and has an increased market demand year by year along with the development of high and new electronic technologies and medicines.
The capacity of a common dicyandiamide production device in China is about 20 million tons/year, the main quality index is that the content is 99.5 percent, the calcium content is 200ppm, the capacity of electronic grade dicyandiamide is about 1 million tons/year, and the main quality index is that the content is 99.8 percent, and the calcium content is 25 ppm.
The original production process technology of the electronic grade dicyandiamide is to dissolve, filter and crystallize the industrial grade dicyandiamide, and has long process route, large equipment investment and high production cost.
The main factors influencing the quality index of the dicyandiamide are impurities such as calcium oxide, calcium hydroxide, calcium carbonate and the like contained in the product, and the calcium-containing impurities in the cyanamide liquid in the production process of the dicyandiamide are removed, so that the amount of the calcium-containing impurities in the crystallized dicyandiamide product can be reduced, and the quality of the dicyandiamide product is improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of dicyandiamide.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a preparation method of dicyandiamide, which comprises the following steps:
s1, mixing lime nitrogen, water and carbon dioxide, and hydrolyzing and carbonizing to produce cyanamide aqueous solution.
S2, heating and polymerizing the aqueous solution of the cyanamide to produce the aqueous solution of the dicyandiamide.
And S3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into the dicyandiamide solution, and flocculating and filtering impurities.
S4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product.
Further, step S1 is specifically: adding lime nitrogen and water into a slurry preparation kettle, hydrolyzing the lime nitrogen to generate a calcium cyanamide solution, adding carbon dioxide gas into a carbonization kettle, and carbonizing the calcium cyanamide into a cyanamide solution.
Further, in step S1, the lime nitrogen is 15 to 20 parts by mass, and the water is 100 to 120 parts by mass.
Further, in step S3, the polyacrylamide is 0.010 to 0.015 parts by mass, and the polyethyleneimine is 0.015 to 0.022 parts by mass.
The invention has the following beneficial effects:
the invention adopts a production process of the composite flocculant taking polyacrylamide and polyethyleneimine as materials, adds the composite flocculant into dicyandiamide solution, performs flocculation precipitation and filtration removal on calcium-containing impurities in the dicyandiamide solution, obviously improves the quality of dicyandiamide, and meets the quality requirement of electronic grade dicyandiamide.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1
A method for preparing dicyandiamide, which comprises the following steps:
s1, adding lime nitrogen and water into a slurry preparation kettle, hydrolyzing the lime nitrogen to generate a calcium cyanamide solution, adding carbon dioxide gas into a carbonization kettle, and carbonizing the calcium cyanamide into a cyanamide solution; the mass portion of the lime nitrogen is 15g, and the mass portion of the water is 100 g.
S2, heating and polymerizing the aqueous solution of the cyanamide to produce the aqueous solution of the dicyandiamide.
S3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into a dicyandiamide solution, and flocculating and filtering impurities; the mass portion of the polyacrylamide is 0.01g, and the mass portion of the polyethyleneimine is 0.015 g;
s4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product.
Through determination, the purity of the prepared dicyandiamide answers 99.8 percent and the calcium content is 20 ppm.
Embodiment 2 a method for preparing dicyandiamide, which includes the steps of:
s1, adding lime nitrogen and water into a slurry preparation kettle, hydrolyzing the lime nitrogen to generate a calcium cyanamide solution, adding carbon dioxide gas into a carbonization kettle, and carbonizing the calcium cyanamide into a cyanamide solution; the mass portion of the lime nitrogen is 20g, and the mass portion of the water is 120 g.
S2, heating and polymerizing the aqueous solution of the cyanamide to produce the aqueous solution of the dicyandiamide.
S3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into a dicyandiamide solution, and flocculating and filtering impurities; the mass portion of the polyacrylamide is 0.015g, and the mass portion of the polyethyleneimine is 0.22 g;
s4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product.
The purity of the prepared dicyandiamide answers 99.7% and the prepared dicyandiamide contains 22ppm of calcium.
Example 3
A method for preparing dicyandiamide, which comprises the following steps:
s1, adding lime nitrogen and water into a slurry preparation kettle, hydrolyzing the lime nitrogen to generate a calcium cyanamide solution, adding carbon dioxide gas into a carbonization kettle, and carbonizing the calcium cyanamide into a cyanamide solution; the mass portion of the lime nitrogen is 18g, and the mass portion of the water is 110 g.
S2, heating and polymerizing the aqueous solution of the cyanamide to produce the aqueous solution of the dicyandiamide.
S3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into a dicyandiamide solution, and flocculating and filtering impurities; the weight portion of the polyacrylamide is 0.013g, and the weight portion of the polyethyleneimine is 0.018 g.
S4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product.
The purity of the prepared dicyandiamide answers 99.8% and the prepared dicyandiamide contains 21ppm of calcium.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and modifications can be made, and equivalents can be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The preparation method of dicyandiamide is characterized by comprising the following steps:
s1, mixing lime nitrogen, water and carbon dioxide, and hydrolyzing and carbonizing to produce cyanamide aqueous solution.
S2, heating and polymerizing the aqueous solution of the cyanamide to produce the aqueous solution of the dicyandiamide.
And S3, adding a trace amount of polyacrylamide and polyethyleneimine composite flocculant into the dicyandiamide solution, and flocculating and filtering impurities.
S4, crystallizing the dicyandiamide aqueous solution, dehydrating, drying and packaging to obtain the product.
2. The method for preparing dicyandiamide according to claim 1, wherein step S1 specifically includes: adding lime nitrogen and water into a slurry preparation kettle, hydrolyzing the lime nitrogen to generate a calcium cyanamide solution, adding carbon dioxide gas into a carbonization kettle, and carbonizing the calcium cyanamide into a cyanamide solution.
3. The method for producing dicyandiamide according to claim 1, wherein in step S1, lime nitrogen is 15 to 20 parts by mass, and water is 100 to 120 parts by mass.
4. The method for producing dicyandiamide according to claim 1, wherein in step S3, the polyacrylamide is 0.010 to 0.015 parts by mass, and the polyethyleneimine is 0.015 to 0.022 parts by mass.
5. The method according to claim 4, wherein in step S3, the polyacrylamide is 0.012 parts by mass and the polyethyleneimine is 0.018 parts by mass.
Priority Applications (1)
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| CN201911419286.6A CN111056977A (en) | 2019-12-31 | 2019-12-31 | Preparation method of dicyandiamide |
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| CN201911419286.6A CN111056977A (en) | 2019-12-31 | 2019-12-31 | Preparation method of dicyandiamide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848458A (en) * | 2020-08-05 | 2020-10-30 | 原平市同利化工有限责任公司 | Process for extracting dicyandiamide in process of preparing 3-mercaptopropionic acid |
| CN112209857A (en) * | 2020-10-29 | 2021-01-12 | 宁夏蓝白黑循环科技有限公司 | Preparation method of dicyandiamide |
| CN112457220A (en) * | 2020-10-26 | 2021-03-09 | 石嘴山市鹏盛化工有限公司 | One-step process for producing electronic grade dicyandiamide |
| CN116751478A (en) * | 2023-06-16 | 2023-09-15 | 江苏云合新材料科技有限公司 | Environment-friendly antibacterial printing ink for tipping paper for cigarettes and preparation method thereof |
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| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method of preparing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by calcium cyanamide |
| CN102010094A (en) * | 2009-09-07 | 2011-04-13 | 中国石油化工股份有限公司 | Method for treating high-calcium and high-salt industrial wastewater |
| CN102167671A (en) * | 2010-12-31 | 2011-08-31 | 张胜勇 | Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue |
| CN103818940A (en) * | 2013-12-30 | 2014-05-28 | 中国神华能源股份有限公司 | Method for decalcifying aluminum chloride and method for extracting aluminum oxide from coal ash |
| CN105294509A (en) * | 2015-12-07 | 2016-02-03 | 上海弗鲁克科技发展有限公司 | System and method for synthesizing dicyandiamide by one-step process |
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2019
- 2019-12-31 CN CN201911419286.6A patent/CN111056977A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method of preparing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by calcium cyanamide |
| CN102010094A (en) * | 2009-09-07 | 2011-04-13 | 中国石油化工股份有限公司 | Method for treating high-calcium and high-salt industrial wastewater |
| CN102167671A (en) * | 2010-12-31 | 2011-08-31 | 张胜勇 | Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue |
| CN103818940A (en) * | 2013-12-30 | 2014-05-28 | 中国神华能源股份有限公司 | Method for decalcifying aluminum chloride and method for extracting aluminum oxide from coal ash |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848458A (en) * | 2020-08-05 | 2020-10-30 | 原平市同利化工有限责任公司 | Process for extracting dicyandiamide in process of preparing 3-mercaptopropionic acid |
| CN111848458B (en) * | 2020-08-05 | 2022-04-26 | 原平市同利化工有限责任公司 | Process for extracting dicyandiamide in process of preparing 3-mercaptopropionic acid |
| CN112457220A (en) * | 2020-10-26 | 2021-03-09 | 石嘴山市鹏盛化工有限公司 | One-step process for producing electronic grade dicyandiamide |
| CN112209857A (en) * | 2020-10-29 | 2021-01-12 | 宁夏蓝白黑循环科技有限公司 | Preparation method of dicyandiamide |
| CN116751478A (en) * | 2023-06-16 | 2023-09-15 | 江苏云合新材料科技有限公司 | Environment-friendly antibacterial printing ink for tipping paper for cigarettes and preparation method thereof |
| CN116751478B (en) * | 2023-06-16 | 2023-12-15 | 江苏云合新材料科技有限公司 | Environment-friendly antibacterial printing ink for tipping paper for cigarettes and preparation method thereof |
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Application publication date: 20200424 |