CN100572359C - The novel high pressure alkali fusion production process of H acid - Google Patents
The novel high pressure alkali fusion production process of H acid Download PDFInfo
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- CN100572359C CN100572359C CNB2008101697239A CN200810169723A CN100572359C CN 100572359 C CN100572359 C CN 100572359C CN B2008101697239 A CNB2008101697239 A CN B2008101697239A CN 200810169723 A CN200810169723 A CN 200810169723A CN 100572359 C CN100572359 C CN 100572359C
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Abstract
The present invention relates to a kind of novel high pressure alkali fusion production process of H acid, belong to H acid high pressure alkali fusion production technique field.This process using is pressed mass ratio with the T acid solution of the liquid caustic soda of 75% concentration and 20% in alkal melting pan 1: 4～1: 5 mixed, under 80～120 ℃ of temperature, dewater, dehydration was held time 3～5 hours, at the uniform velocity adding in the alkal melting pan with T acid mass ratio is 1: 0.1～1: 0.2 solvent again, temperature in the alkal melting pan is risen to 150～180 ℃, pot inner pressure rises to 2.0～3.0MPa, keep this temperature and pressure reaction 1 hour, reaction generates H acid suspended substance, after filtration, obtain finished product H acid after the drying.The present invention can bring up to 86% by original 74% with alkali fusion thing HPLC content, and final product quality is greatly improved, amino value 〉=86%, HPLC content 〉=97%, T acid≤0.5%, chromotropic acid≤1.5%, and this technological reaction is stable.
Description
Technical field:
The present invention relates to a kind of novel high pressure alkali fusion production process of H acid, belong to H acid high pressure alkali fusion production technique field.
Background technology:
H acid is a kind of special-purpose intermediate of making dyestuff, is widely used in industries such as printing and dyeing, weaving, chemical industry.The molten production technique of common H soda acid is in reactor, viscosity after T acid is dewatered with NaOH is high, when closing the pot reaction with this understanding, reaction pressure is 0.5～1.0Mpa, because the requirement temperature of reaction must be more than 210 ℃ when low pressure reaction, too high temperature of reaction can cause some production of by-products again, because of material extreme thickness, causes reaction to have local unbalanced phenomenon simultaneously.Therefore the yield that adopts this method production is below 75%, and by-products content is higher in addition simultaneously, and particularly the chromatogram content of chromotropic acid is up to more than 10%, and these by products can have a strong impact on the quality and the yield of the finished product H acid product.
Summary of the invention:
The objective of the invention is to: a kind of low cost is provided, and the novel high pressure alkali fusion production process of high-quality H acid can effectively improve the yield of alkali fusion reaction, reduces production of by-products simultaneously, and the raw materials consumption that high-quality H acid is produced reduces, and quality product improves.
The present invention realizes above-mentioned purpose by the following technical solutions:
A kind of novel high pressure alkali fusion production process of H acid is characterized in that it comprises the steps:
(1) batching: in the liquid caustic soda suction alkal melting pan with 75% concentration,, add back unlatching stirrer and mix in the T acid solution of 1: 4～1: 5 ratio of mass ratio adding content 20%;
(2) dehydration: open alkal melting pan jacket steam device the temperature in the alkal melting pan is warming up to 80～120 ℃, the valve of opening again on the dehydration pipeline begins dehydration, and the water vapor of deviating from is through condenser condenses; Dewatering time 3～5 hours;
(3) solubilizing agent: open and add the solvent pipe valve, at the uniform velocity add in the alkal melting pan and T acid solution mass ratio is 1: 0.1～1: 0.2 a methyl alcohol;
(4) reaction: open alkal melting pan jacket steam device, the temperature in the alkal melting pan is risen to 150～180 ℃, solvent evaporates, pot inner pressure rises to 2.0～3.0MPa, keeps this temperature and pressure reaction 1 hour;
(5) reclaim: open the valve of solvent, solvent enters the basin recycle after the condenser cooling;
(6) segregation: 20% the dilute sulphuric acid reaction that sampling analysis H acid content, the alkali fusion material after qualified join in the segregation pot with 2～4 times of volumes generates H acid suspended substance, after filtration, after the drying finished product H acid.
The present invention's advantage compared with prior art is:
Adopt technology of the present invention, alkali fusion thing HPLC content during H acid is produced has been brought up to more than 86% by original 74%, and final product quality is greatly improved, the amino value 〉=86% of finished product, HPLC content 〉=97%, T acid≤0.5%, chromotropic acid≤1.5%, and this technological reaction is stablized feasible.
Embodiment:
(is that the sodium hydroxide liquid caustic soda of 75% concentration is an example with 1000kg content)
The first step: with content be 30% or 48% liquid caustic soda by concentration and evaporation moisture content, obtain 75% high temperature liquid caustic soda, 75% liquid caustic soda is stored in the basin that has the steam insulation chuck; T acid solution with 20% is stored in the stainless steel scale tank that has the steam insulation chuck.
Second step: the sodium hydroxide that in the reactor of stirrer is housed, in the alkali fusion reactor, adds 1000kg75% concentration by under meter.After adding alkali and finishing, slowly add the T acid solution of 4300kg content 20%, add the back and open stirrer and mix.
The 3rd step: open alkal melting pan jacket steam device the temperature in the alkal melting pan is warming up to 80～120 ℃, the valve of opening again on the dehydration pipeline begins dehydration, and the water vapor of deviating from enters scale tank after condenser condenses; After dewatering time is kept 4 hours, close the valve on the dehydrated tube, finish dehydration.
The 4th step: open the valve of the enterprising solvent of alkali fusion reactor, in the alkali fusion reactor, add methyl alcohol 580kg, add all valves on the off-response still of back by high-pressure pump.The 5th step: according to reactor temperature, regulate the aperture of chuck steam valve, temperature of reaction kettle is risen to more than 150 ℃, controlled temperature is at 180 ℃, and pressure 2.8MPa keeps reaction 1 hour.
The 6th step: slowly open the valve of solvent, solvent vapour enters condenser after decompression, become liquid by condensation, and question response still internal pressure is closed the desolventizing valve after reducing to normal pressure, and recovered solvent enters the solvent tanker recycle.
The 7th step: sampling analysis H acid content, it is that qualified, qualified alkali fusion thing changes the storage of alkali fusion thing storage tank over to greater than 86% that HPLC analyzes alkali fusion thing H acid content.Qualified alkali fusion thing joins in the segregation pot 20% dilute sulphuric acid reaction with 2～4 times of volumes in next step operation, after filtration, after the drying H acid finished product 650Kg.
Claims (1)
1, a kind of novel high pressure alkali fusion production process of H acid is characterized in that, it comprises the steps:
(1) batching: in the liquid caustic soda suction alkal melting pan with 75% concentration,, add back unlatching stirrer and mix in the T acid solution of 1: 4～1: 5 ratio of mass ratio adding content 20%;
(2) dehydration: open alkal melting pan jacket steam device the temperature in the alkal melting pan is warming up to 80～120 ℃, the valve of opening again on the dehydration pipeline begins dehydration, and the water vapor of deviating from is through condenser condenses; Dewatering time 3～5 hours;
(3) solubilizing agent: open and add the solvent pipe valve, at the uniform velocity add in the alkal melting pan and T acid solution mass ratio is 1: 0.1～1: 0.2 a methyl alcohol;
(4) reaction: open alkal melting pan jacket steam device, the temperature in the alkal melting pan is risen to 150～180 ℃, solvent evaporates, pot inner pressure rises to 2.0～3.0MPa, keeps this temperature and pressure reaction 1 hour;
(5) reclaim: open the valve of solvent, solvent enters the basin recycle after the condenser cooling;
(6) segregation: 20% the dilute sulphuric acid reaction that sampling analysis H acid content, the alkali fusion material after qualified join in the segregation pot with 2～4 times of volumes generates H acid suspended substance, after filtration, after the drying finished product H acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2008101697239A CN100572359C (en) | 2008-10-15 | 2008-10-15 | The novel high pressure alkali fusion production process of H acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2008101697239A CN100572359C (en) | 2008-10-15 | 2008-10-15 | The novel high pressure alkali fusion production process of H acid |
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| CN101367752A CN101367752A (en) | 2009-02-18 |
| CN100572359C true CN100572359C (en) | 2009-12-23 |
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| CNB2008101697239A Active CN100572359C (en) | 2008-10-15 | 2008-10-15 | The novel high pressure alkali fusion production process of H acid |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748901B (en) * | 2015-11-25 | 2018-11-06 | 江苏扬农化工集团有限公司 | A kind of alkali fusion and aftertreatment technology of H acid |
| CN105669500A (en) * | 2016-02-29 | 2016-06-15 | 江苏吉华化工有限公司 | Method adopting clean process for preparing H-acid |
| CN106006676B (en) * | 2016-04-08 | 2017-05-31 | 江苏扬农化工集团有限公司 | A kind of method of NaOH in recovery H soda acid process of smelting |
| CN108191715A (en) * | 2017-11-27 | 2018-06-22 | 江苏力禾颜料有限公司 | High pressure alkali fusion preparation process |
| CN108003071A (en) * | 2017-12-04 | 2018-05-08 | 大柴旦乐青科技化学有限公司 | A kind of H acid high pressure alkali fusion technique |
| CN109096154A (en) * | 2018-08-16 | 2018-12-28 | 山东裕源集团有限公司 | A kind of H acid production process |
| CN109651207A (en) * | 2019-01-09 | 2019-04-19 | 江苏吉华化工有限公司 | A kind of T soda acid melts the solution and method of reduction Freund acid generation in reaction |
-
2008
- 2008-10-15 CN CNB2008101697239A patent/CN100572359C/en active Active
Non-Patent Citations (2)
| Title |
|---|
| T酸碱熔制备H酸的新工艺. 彭友谊等.染料工业，第36卷第3期. 1999 |
| T酸碱熔制备H酸的新工艺. 彭友谊等.染料工业，第36卷第3期. 1999 * |
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| CN101367752A (en) | 2009-02-18 |
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Owner name: CHUYUAN HIGH-NEW TECHNOLOGY GROUP CO., LTD. Free format text: FORMER OWNER: HUBEI CHUYUAN CHEMICAL CO., LTD. Effective date: 20120829 |
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Effective date of registration: 20120829 Address after: 434400 Hubei province Shishou City High-tech Park Patentee after: Chuyuan High-New Technology Group Co., Ltd. Address before: 434400 Hubei province Shishou City Zhang Huan high tech Park Patentee before: Hubei Chuyuan Chemical Co., Ltd. |