CN103408408A - Method and equipment for recovering byproduct dimethoxymethane generated in production of glyphosate raw medicine through glycine method - Google Patents
Method and equipment for recovering byproduct dimethoxymethane generated in production of glyphosate raw medicine through glycine method Download PDFInfo
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- CN103408408A CN103408408A CN2013103796988A CN201310379698A CN103408408A CN 103408408 A CN103408408 A CN 103408408A CN 2013103796988 A CN2013103796988 A CN 2013103796988A CN 201310379698 A CN201310379698 A CN 201310379698A CN 103408408 A CN103408408 A CN 103408408A
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Abstract
The invention aims to provide a method for recovering byproduct dimethoxymethane generated in production of a glyphosate raw medicine through a glycine method. According to the method, the physical and chemical properties of dimethoxymethane are used, and the byproduct dimethoxymethane generated in production of glyphosate is further condensed and recovered by adopting a multistage condensation method. Specifically, a lot of generated dimethoxymethane materials are sequentially subjected to first-stage condensate water pre-cooling recovery, second-stage ice brine cooling recovery and third-stage ice brine deep cooling recovery, and then are recovered by rectifying in a rectifying column. By adopting the method and the equipment, the recovery rate of the dimethoxymethane is improved to be more than 99.5%, the economic benefit and cost are significantly controlled, the environmental pollution is greatly reduced, and the economic benefit is greatly improved.
Description
Technical field
The present invention relates to recovery method and the retrieving arrangement of by product methylal〔Su〕 in the former medicine of a kind of producing glyphosate by using glycine, through three grades of condensations, improve the rate of recovery of methylal〔Su〕.
Background technology
In recent years, domestic glyphosate market great waves were indefinite.The glyphosate average price only had 2.8 ten thousand yuan/tons in 2006, and entered glyphosate prices in 2007 continuous rise just as wild chargers, the highlyest once reached 100,000 yuan/tons.To reproduce and will increase newly the appearance of device message in May, 2008 along with About Monsanto Chemicals declaration shutdown device, domestic small business is busy with arbitrage and sells off at a low price, and its a price also road is descending.Industry is after producing releasable impact and shuffling in a short time, and industry development and the level of profitability have returned rationality.Therefore, production control cost, autonomous innovation, dwindle the production technology gap with overseas enterprise, just can make enterprise have at any time competitive power.Glyphosate technicals is a kind of non-volatile white solid powder, and moisture 10-20%, to people and animals' low toxicity; Methylal〔Su〕 is the volatile flammable liquid of achromaticity and clarification, and chloroform smell and pungent taste are arranged, and can do efficient solvent, fusing point-104.8 ℃, 42.3 ℃ of boiling points.Manufacturer for glyphosate technicals, what majority adopted is traditional glycine method production technique, what existing recovery methylal〔Su〕 method adopted is after the dealcoholysis stage obtains the methylal〔Su〕 phlegma with cooling by water recovery tail gas, to carry out rectifying through rectifying tower to reclaim methylal〔Su〕, its shortcoming is that methylal〔Su〕 condensation recovery is insufficient, and the rate of recovery only has 80%.
Summary of the invention
The object of the present invention is to provide the recovery method of by product methylal〔Su〕 in the former medicine of a kind of producing glyphosate by using glycine, utilize the physico-chemical property of methylal〔Su〕, adopt the multi-stage condensing method that the further condensation of by product methylal〔Su〕 in glyphosate production process is reclaimed.
The present invention realizes above-mentioned purpose like this: at methanol solvate, under the effect of Triethylamine catalyst, drop into paraformaldehyde, glycine, dimethylphosphite carries out depolymerization, addition, condensation reaction, after hydrochloric acid intensification dealcoholysis, in the dealcoholysis operation, can produce a large amount of methylal〔Su〕 air scavenge, this technology utilizes the methylal〔Su〕 material characteristic to reclaim on basis in water-cooled, increase again two-stage salt cold, be that first step water of condensation condensation (temperature is controlled 0-5 ℃) is carried out the precooling recovery to methylal〔Su〕 gas, most of methylal〔Su〕 condensation is reclaimed in second stage icy salt solution condensation (1--10 ℃), third stage icy salt solution condensation deep cooling (10--20 ℃) contains a small amount of methylal〔Su〕 tail gas cryogenic by residue and reclaims.The methylal〔Su〕 phlegma of three grades of recovery is collected by the condensed fluid collection basin, is delivered to the methylal〔Su〕 rectifying tower and carries out the rectifying recovery.
Another object of the present invention is to provide the recovery system of by product methylal〔Su〕 in the former medicine of a kind of producing glyphosate by using glycine, adopt the multi-stage condensing device that the further condensation of by product methylal〔Su〕 in glyphosate production process is reclaimed.
The present invention realizes above-mentioned purpose like this: the synthesis reaction vessel bottom is connected with dealcoholysis still top by pump, dealcoholysis still bottom leads to the glyphosate synthesis operation, dealcoholysis still top is the one-level water of condensation condenser through connecting successively, secondary icy salt solution condenser, three grades of icy salt solution condensers, again by one-level water of condensation condenser, secondary icy salt solution condenser, the condenser bottom of three grades of icy salt solution condensers passes into methylal〔Su〕 condenser storage tank, methylal〔Su〕 condenser storage tank is squeezed into methylal〔Su〕 rectifying tower top by pump, and the rectifying tower bottom leads to the methylal〔Su〕 finished product storage tank.
Advantage of the present invention: solved in glyphosate production process the problems such as the methylal〔Su〕 rate of recovery is low, the wasting of resources, contaminate environment, guaranteed the equipment smooth running, optimized production process and operating environment, enhance productivity, the methylal〔Su〕 rate of recovery is brought up to more than 99.5%, economic benefit and cost control are remarkable, have greatly reduced environmental pollution and have increased economic efficiency.
The accompanying drawing explanation
Fig. 1 is the recovery process equipment of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine.
1. synthesis reaction vessels wherein, 2. dealcoholysis still, 3. one-level water of condensation condenser, 4. secondary icy salt solution condenser, 5. three grades of icy salt solution condensers, 6. rectifying tower, 7. condenser storage tank, 8. finished product storage tank, 9-1,2. pump.
Embodiment
At methanol solvate, under the effect of Triethylamine catalyst, to glyphosate synthesis reactor 1, drop into paraformaldehyde, glycine, dimethylphosphite carries out depolymerization, addition, condensation reaction, reaction solution is squeezed in dealcoholysis still 2 through pump 9-1, after toward dealcoholysis still 2, adding hydrochloric acid intensification dealcoholysis, produce a large amount of methylal〔Su〕 gas, the interior methylal〔Su〕 material of dealcoholysis still 2 reclaims through one-level water of condensation condenser 3 precoolings of 0-5 ℃ successively,-1--10 ℃ of secondary icy salt solution condenser 4 cooling recovery, after reclaiming ,-10--20 ℃ of three grades of icy salt solution condensers, 5 deep coolings pass into methylal〔Su〕 condensation storage tank 7, methylal〔Su〕 is squeezed into after rectifying tower 6 rectifying are reclaimed and is obtained the finished product methylal〔Su〕 through pump 9-2.
Concrete technology equipment is:
Claims (5)
1. the recovery method of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine, under the effect of methanol solvate, Triethylamine catalyst, input paraformaldehyde, glycine, dimethylphosphite carry out depolymerization, addition, condensation reaction, after hydrochloric acid intensification dealcoholysis, produce a large amount of methylal〔Su〕 gas, it is characterized in that: the methylal〔Su〕 material reclaims through the precooling of one-level water of condensation successively, the cooling recovery of secondary icy salt solution, and three grades of icy salt solution deep coolings reclaim and reclaim by rectifying tower rectifying.
2. the recovery method of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine according to claim 1, it is characterized in that: the temperature of one-level water of condensation is 0-5 ℃.
3. the recovery method of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine according to claim 1 is characterized in that: the temperature of secondary icy salt solution is-1--10 ℃.
4. the recovery method of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine according to claim 1 is characterized in that: the temperature of three grades of icy salt solutions is-10--20 ℃.
5. the recovery system of by product methylal〔Su〕 in the former medicine of producing glyphosate by using glycine, synthesis reaction vessel bottom (1) is connected with dealcoholysis still top (2) by pump (9-1), dealcoholysis still bottom leads to the glyphosate Crystallization Procedure, it is characterized in that: dealcoholysis still top (2) is the one-level water of condensation condenser (3) through connecting successively, secondary icy salt solution condenser (4), three grades of icy salt solution condensers (5), again by one-level water of condensation condenser (3), secondary icy salt solution condenser (4), the condenser bottom of three grades of icy salt solution condensers (5) passes into methylal〔Su〕 condenser storage tank (7), methylal〔Su〕 condenser storage tank (7) is squeezed into methylal〔Su〕 rectifying tower top (6) by pump (9-2), the rectifying tower bottom leads to methylal〔Su〕 finished product storage tank (8).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103796988A CN103408408A (en) | 2013-08-28 | 2013-08-28 | Method and equipment for recovering byproduct dimethoxymethane generated in production of glyphosate raw medicine through glycine method |
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| CN2013103796988A CN103408408A (en) | 2013-08-28 | 2013-08-28 | Method and equipment for recovering byproduct dimethoxymethane generated in production of glyphosate raw medicine through glycine method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163832A (en) * | 2014-08-12 | 2014-11-26 | 湖北泰盛化工有限公司 | Glyphosate continuous production device and glyphosate continuous production method |
| CN105737457A (en) * | 2016-03-08 | 2016-07-06 | 曲靖众一精细化工股份有限公司 | Solvent recovery technology |
| CN106278833A (en) * | 2016-08-13 | 2017-01-04 | 安徽东至广信农化有限公司 | The recovery method of dimethoxym ethane in a kind of glyphosate production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977137A (en) * | 2012-11-29 | 2013-03-20 | 湖北泰盛化工有限公司 | Condensate recovery method for glyphosate synthesis solution |
| CN103113403A (en) * | 2013-02-06 | 2013-05-22 | 湖北泰盛化工有限公司 | Glyphosate de-acidifying device and de-acidifying device method |
-
2013
- 2013-08-28 CN CN2013103796988A patent/CN103408408A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977137A (en) * | 2012-11-29 | 2013-03-20 | 湖北泰盛化工有限公司 | Condensate recovery method for glyphosate synthesis solution |
| CN103113403A (en) * | 2013-02-06 | 2013-05-22 | 湖北泰盛化工有限公司 | Glyphosate de-acidifying device and de-acidifying device method |
Non-Patent Citations (1)
| Title |
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| 陈万福: "草甘膦生产中溶剂分离回收的新工艺", 《农药》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163832A (en) * | 2014-08-12 | 2014-11-26 | 湖北泰盛化工有限公司 | Glyphosate continuous production device and glyphosate continuous production method |
| CN105737457A (en) * | 2016-03-08 | 2016-07-06 | 曲靖众一精细化工股份有限公司 | Solvent recovery technology |
| CN105737457B (en) * | 2016-03-08 | 2018-08-14 | 曲靖众一精细化工股份有限公司 | A kind of solvent recovery process |
| CN106278833A (en) * | 2016-08-13 | 2017-01-04 | 安徽东至广信农化有限公司 | The recovery method of dimethoxym ethane in a kind of glyphosate production |
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Application publication date: 20131127 |