CN102167671A - Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue - Google Patents
Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue Download PDFInfo
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- CN102167671A CN102167671A CN2010106155046A CN201010615504A CN102167671A CN 102167671 A CN102167671 A CN 102167671A CN 2010106155046 A CN2010106155046 A CN 2010106155046A CN 201010615504 A CN201010615504 A CN 201010615504A CN 102167671 A CN102167671 A CN 102167671A
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- charcoal
- dicyandiamide
- calcium
- calcium sulfate
- aqueous solution
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Abstract
The invention provides a method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue. In the invention, by mixing the dicyandiamide waste residue with water and separating the part which can not be dissolved in water, hydrogen cyanamide aqueous solution as well as a mixture of calcium sulfate and charcoal are obtained; by binary-polymerizing the hydrogen cyanamide aqueous solution, the dicyandiamide is obtained; by adequately reacting the mixture of calcium sulfate and charcoal with excessive dilute hydrochloric acid, calcium chloride solution and charcoal filter cakes are obtained; by washing the charcoal filter cakes, then drying and crushing, the industrial charcoal is obtained; by adequately reacting the calcium chloride solution with sulfuric acid and then filtering, calcium sulfate precipitation and hydrochloric acid solution are obtained; by drying and then crushing the calcium sulfate precipitation, sulfate precipitation product is obtained. The method in the invention is simple and requires low equipment investment. And with the method, the yield rate of product is high. Therefore, the method in the invention provides good economic and environment benefits.
Description
Technical field
The present invention relates to the comprehensive utilization of three industrial wastes dicyandiamide sludge as material and administer technical field, particularly, relate to a kind of method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal.
Background technology
The lime nitrogen method is hydrolyzed lime nitrogen and water, the cyanogen ammonia hydrogen calcium hydrolyzed solution of reaction gained suspension, remove the calcium hydroxide filter residue through filtration under diminished pressure, the logical people's filtrate of carbonic acid gas that decomposition of limestone produces is carried out the decalcification reaction, generate the cyanogen ammoniacal liquor, polymerization under alkaline condition more after filtration, crystallisation by cooling, separation, drying, makes Dyhard RU 100.Its chemical equation is:
2CaCN
2+2H
2O→Ca(HCN
2)
2+Ca(OH)
2
Ca(HCN
2)
2+CO
2+H
2O→2NH
2CN+CaCO
3
2NH
2CN→(NH
2CN)
2
By the production technique and the measuring of above Dyhard RU 100, dicyandiamide sludge as material mainly consist of lime carbonate, charcoal and cyanamide.For a long time, dicyandiamide sludge as material is mainly with making cement with in order to improving the soil, or stacks arbitrarily, not only wastes raw material, also contaminate environment.
People also actively seek the comprehensive regulation of dicyandiamide sludge as material and utilize method, as application number is 00113513.9, Chinese patent utilize dicyandiamide sludge as material to produce lime, application number is that 200410022909.3 Chinese patent utilizes dicyandiamide sludge as material to produce solid fuel, yet, these patents have all only been utilized the minority effective constituent in the dicyandiamide sludge as material, do not give full play to the function of dicyandiamide sludge as material.
Summary of the invention
For this reason, the application provides a kind of method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal, and lime carbonate in the dicyandiamide sludge as material, charcoal element and cyanamide are fully excavated and utilized to this method, realized turning waste into wealth, for the comprehensive utilization of dicyandiamide sludge as material provides new way.
Technical scheme of the present invention is as follows: a kind of method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal comprises following concrete steps:
(1) with described dicyandiamide sludge as material with after water mixes, separation can not be dissolved part, obtains the cyanamide aqueous solution, and the mixture of lime carbonate and charcoal, also contains a spot of silicate in this mixture;
(2) the described cyanamide aqueous solution is carried out the binary polymerization, obtain the Dyhard RU 100 product;
(3) mixture and the excessive dilute hydrochloric acid with described lime carbonate and charcoal fully reacts, and at this moment, lime carbonate and hydrochloric acid reaction generate calcium chloride and CO
2Gas, and charcoal not with hydrochloric acid reaction, can not be water-soluble and precipitate, filtering reacting liquid obtains calcium chloride solution and charcoal filter cake;
(4) obtain industrial charcoal after charcoal filter cake washing, drying, the pulverizing;
(5) calcium chloride filtrate and dilute sulphuric acid are fully reacted after-filtration, obtain calcium sulfate precipitation and hydrochloric acid soln; Calcium sulfate precipitation washing, drying after the pulverizing, obtain the calcium sulfate product.
The pH that regulates the described cyanamide aqueous solution aqueous solution carries out the binary polyreaction again for alkalescence, and its temperature of reaction is 120 ℃.
It is 3%～30% that the amount of the water that step (1) is used should make the concentration of the cyanamide aqueous solution that obtains.
The hydrochloric acid soln of step (1) gained returns step (3) recycle.
The method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial calcium chloride and charcoal of the present invention, its method is simple, and facility investment is few, and the efficiency of pcr product height has good economic benefit and environmental benefit.
Embodiment
Embodiment 1:
A kind of method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal comprises following concrete steps:
(1) weighing dicyandiamide sludge as material 500kg, with after water mixes, separation can not be dissolved part with described dicyandiamide sludge as material, and the amount of institute's water should satisfy that to obtain mass concentration be 3% the cyanamide aqueous solution, and the mixture of lime carbonate and charcoal, also contain a spot of silicate in this mixture;
(2) pH that regulates the described cyanamide aqueous solution aqueous solution be alkaline, and the described cyanamide aqueous solution is carried out the binary polymerization in 120 ℃, obtains the Dyhard RU 100 product;
(3) mixture and the excessive dilute hydrochloric acid with described lime carbonate and charcoal fully reacts, and at this moment, lime carbonate and hydrochloric acid reaction generate calcium chloride and CO
2Gas, and charcoal not with hydrochloric acid reaction, can not be water-soluble and precipitate, filtering reacting liquid obtains calcium chloride solution and charcoal filter cake;
(4) obtain industrial charcoal after charcoal filter cake washing, drying, the pulverizing;
(5) calcium chloride filtrate and dilute sulphuric acid are fully reacted after-filtration, obtain calcium sulfate precipitation and hydrochloric acid soln; Calcium sulfate precipitation washing, drying after the pulverizing, obtain the calcium sulfate product.
Embodiment 1:
A kind of method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal comprises following concrete steps:
(1) weighing dicyandiamide sludge as material 500kg, with after water mixes, separation can not be dissolved part with described dicyandiamide sludge as material, and the amount of institute's water should satisfy that to obtain mass concentration be 30% the cyanamide aqueous solution, and the mixture of lime carbonate and charcoal, also contain a spot of silicate in this mixture;
(2) pH that regulates the described cyanamide aqueous solution aqueous solution be alkaline, and the described cyanamide aqueous solution is carried out the binary polymerization in 120 ℃, obtains the Dyhard RU 100 product;
(3) mixture and the excessive dilute hydrochloric acid with described lime carbonate and charcoal fully reacts, and at this moment, lime carbonate and hydrochloric acid reaction generate calcium chloride and CO
2Gas, and charcoal not with hydrochloric acid reaction, can not be water-soluble and precipitate, filtering reacting liquid obtains calcium chloride solution and charcoal filter cake;
(4) obtain industrial charcoal after charcoal filter cake washing, drying, the pulverizing;
(5) calcium chloride filtrate and dilute sulphuric acid are fully reacted after-filtration, obtain calcium sulfate precipitation and hydrochloric acid soln; Calcium sulfate precipitation washing, drying after the pulverizing, obtain the calcium sulfate product.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (4)
1. a method of utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal is characterized in that, this method comprises following concrete steps:
(1) with described dicyandiamide sludge as material with after water mixes, separation can not be dissolved part, obtains the cyanamide aqueous solution, and the mixture of lime carbonate and charcoal, also contains a spot of silicate in this mixture;
(2) the described cyanamide aqueous solution is carried out the binary polymerization, obtain the Dyhard RU 100 product;
(3) mixture and the excessive dilute hydrochloric acid with described lime carbonate and charcoal fully reacts, and filtering reacting liquid obtains calcium chloride solution and charcoal filter cake;
(4) obtain industrial charcoal after charcoal filter cake washing, drying, the pulverizing;
(5) calcium chloride filtrate and dilute sulphuric acid are fully reacted after-filtration, obtain calcium sulfate precipitation and hydrochloric acid soln; Calcium sulfate precipitation washing, drying after the pulverizing, obtain the calcium sulfate product.
2. the method for utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal as claimed in claim 1 is characterized in that, the pH that regulates the described cyanamide aqueous solution aqueous solution carries out the binary polyreaction again for alkalescence, and its temperature of reaction is 120 ℃.
3. the method for utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal as claimed in claim 1 is characterized in that, it is 3%～30% that the amount of the water that step (1) is used should make the concentration of the cyanamide aqueous solution that obtains.
4. the method for utilizing dicyandiamide sludge as material to prepare Dyhard RU 100, industrial sulphuric acid calcium and charcoal as claimed in claim 1 is characterized in that, the hydrochloric acid soln of step (1) gained returns step (3) recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106155046A CN102167671A (en) | 2010-12-31 | 2010-12-31 | Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106155046A CN102167671A (en) | 2010-12-31 | 2010-12-31 | Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue |
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| Publication Number | Publication Date |
|---|---|
| CN102167671A true CN102167671A (en) | 2011-08-31 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106155046A Pending CN102167671A (en) | 2010-12-31 | 2010-12-31 | Method for preparing dicyandiamide, industrial calcium sulfate and charcoal by using dicyandiamide waste residue |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011161A (en) * | 2012-12-19 | 2013-04-03 | 宁夏兴平精细化工股份有限公司 | Comprehensive utilization method of cyanamide waste residue |
| CN103696014A (en) * | 2013-12-12 | 2014-04-02 | 宁夏贝利特化工有限公司 | Method for producing calcium sulfate whisker and calcium sulfate by using wastes produced during production of nitroguanidine and dicyandiamide |
| CN106012012A (en) * | 2016-05-31 | 2016-10-12 | 宁夏大学 | Method for preparing calcium carbonate whiskers from dicyandiamide waste residues |
| CN107189497A (en) * | 2017-06-14 | 2017-09-22 | 神雾科技集团股份有限公司 | The system and method for separating carbon black in lime nitrogen |
| CN111056977A (en) * | 2019-12-31 | 2020-04-24 | 石嘴山市鹏盛化工有限公司 | Preparation method of dicyandiamide |
| CN112642590A (en) * | 2020-12-30 | 2021-04-13 | 宁夏嘉峰化工有限公司 | Hydrodynamic cavitation enhanced cyanamide waste residue flotation separation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB191105713A (en) * | 1910-03-10 | 1911-07-27 | Emil Collett | The Production of Graphite and other By-products in the Manufacture of Ammonia. |
| GB636600A (en) * | 1946-02-15 | 1950-05-03 | Saint Gobain | Method of preparing cyanamide and polymers thereof |
| DE2649404A1 (en) * | 1976-10-29 | 1978-05-03 | Sueddeutsche Kalkstickstoff | Extn. of graphite from residues of calcium cyanamide hydrolysis - by multiple flotation and acid treatment |
| 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 |
-
2010
- 2010-12-31 CN CN2010106155046A patent/CN102167671A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB191105713A (en) * | 1910-03-10 | 1911-07-27 | Emil Collett | The Production of Graphite and other By-products in the Manufacture of Ammonia. |
| GB636600A (en) * | 1946-02-15 | 1950-05-03 | Saint Gobain | Method of preparing cyanamide and polymers thereof |
| DE2649404A1 (en) * | 1976-10-29 | 1978-05-03 | Sueddeutsche Kalkstickstoff | Extn. of graphite from residues of calcium cyanamide hydrolysis - by multiple flotation and acid treatment |
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011161A (en) * | 2012-12-19 | 2013-04-03 | 宁夏兴平精细化工股份有限公司 | Comprehensive utilization method of cyanamide waste residue |
| CN103696014A (en) * | 2013-12-12 | 2014-04-02 | 宁夏贝利特化工有限公司 | Method for producing calcium sulfate whisker and calcium sulfate by using wastes produced during production of nitroguanidine and dicyandiamide |
| CN103696014B (en) * | 2013-12-12 | 2015-12-30 | 宁夏贝利特化工有限公司 | By the method for producing nitroguanidine, the waste of Dyhard RU 100 produces calcium sulfate crystal whiskers and calcium sulfate |
| CN106012012A (en) * | 2016-05-31 | 2016-10-12 | 宁夏大学 | Method for preparing calcium carbonate whiskers from dicyandiamide waste residues |
| CN106012012B (en) * | 2016-05-31 | 2018-10-23 | 宁夏大学 | The method for preparing calcium carbonate crystal whisker with dicyandiamide sludge as material |
| CN107189497A (en) * | 2017-06-14 | 2017-09-22 | 神雾科技集团股份有限公司 | The system and method for separating carbon black in lime nitrogen |
| CN111056977A (en) * | 2019-12-31 | 2020-04-24 | 石嘴山市鹏盛化工有限公司 | Preparation method of dicyandiamide |
| CN112642590A (en) * | 2020-12-30 | 2021-04-13 | 宁夏嘉峰化工有限公司 | Hydrodynamic cavitation enhanced cyanamide waste residue flotation separation method |
| CN112642590B (en) * | 2020-12-30 | 2022-06-03 | 宁夏嘉峰化工有限公司 | Hydrodynamic cavitation enhanced cyanamide waste residue flotation separation method |
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Application publication date: 20110831 |