CN101423532B - Continuous crystallisation process in glyphosate production - Google Patents
Continuous crystallisation process in glyphosate production Download PDFInfo
- Publication number
- CN101423532B CN101423532B CN2008101761057A CN200810176105A CN101423532B CN 101423532 B CN101423532 B CN 101423532B CN 2008101761057 A CN2008101761057 A CN 2008101761057A CN 200810176105 A CN200810176105 A CN 200810176105A CN 101423532 B CN101423532 B CN 101423532B
- Authority
- CN
- China
- Prior art keywords
- glyphosate
- crystallization
- crystallizer
- production
- recycle pump
- Prior art date
- 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.)
- Active
Links
Images
Abstract
The invention discloses a method for continuous crystallization in the production process of glyphosate. After the hydrolysate of an alkyl ester method for preparing glyphosate is neutralized, the neutralized hydrolysate is continuously charged into a circulating type crystallizer for crystallization; the average residence time in the crystallizer is between 0.5 and 24 hours; the crystallization temperature is between 0 and 40 DEG C; and the crystallized liquor after circulating crystallization is continuously discharged and separated. The method can realize the continuous crystallization in the production process of glyphosate, thereby effectively improving the crystallization stability and automaticity in the production process of glyphosate, improving the product quality of glyphosate, and reducing the production cost of glyphosate.
Description
Related application
The present patent application be in the application number that on September 15th, 2006 submitted to Patent Office of China national Department of Intellectual Property be 200610153244.9, denomination of invention divides an application for the application for a patent for invention of " a kind of method of continuous crystallisation in the glyphosate production ".
Technical field
The present invention relates to neutralization continuously in the alkyl esterification method glyphosate production process, crystallization, filtering research field.Relate in particular to and adopt circulating crystallization vat, achieve the method for the neutralization of alkyl esterification method glyphosate, crystallization, filtration serialization production.
Background technology
Glyphosate is the steriland herbicide of a kind of low toxicity, efficient, wide spectrum, at first succeeded in developing by U.S. Monsanto Company in 1974, and in the many national applications in the whole world patent protection.The nineties middle and later periods, along with its patent protection the expiring successively and the extensive plantation of resistance glyphosate transgenic crop of countries in the world, glyphosate is used has been obtained fast development, become the maximum and fastest-rising pesticide species of output.
The synthetic method of glyphosate is a lot, but industrialized operational path is present only with two, i.e. IDA technology and alkyl esterification method technology.Alkyl esterification method technology is the operational path that the most of manufacturing enterprises of China adopt.China generally all is the still formula dimethyl ester method at intermittence that adopts band to stir at present, its level of automation is low, and single covering device ability is little, long reaction time, front and back produce and lack continuity, produce and be subject to artificial factor and the wild effect that occurs now and then, and production efficiency is low, energy utilization is unreasonable, is unfavorable for the scale operation of glyphosate production.
Summary of the invention
At above deficiency, the invention provides the method for continuous crystallisation in a kind of glyphosate production.
The present invention realizes by following technical scheme: the hydrolyzed solution with alkyl esterification method production is neutralized to pH value behind 0.5-6 through adding alkali, preferred 1-2, enter circulating crystallization vat and carry out crystallization, the crystal solution of advantages of good crystallization enters separator continuously, separates to obtain the former powder of glyphosate.
Crystallizer tank all is the mode that adopt to stir in the prior art, and adopting to stir in the large-tonnage device needs the very large power that starts, if adopt a plurality of stirrings then may produce the dead angle again, stirs inhomogeneous.
The crystallization vat is to circulate by recycle pump among the present invention.Adopt many recycle pumps to be distributed in and circulate around the crystallizer tank, make to have formed a more stable solid-liquid current system in the groove and do not precipitate, avoided adopting the many deficiencies that stir.
As shown in Figure 1, in entering with the hydrolyzed solution of alkyl esterification method production and still be neutralized to pH value behind 0.5-6 through adding alkali, preferred 1-2, enter the crystallization vat from the top, neutralizer enters the recycle system from the D point, enter in the groove through circulating-pump outlet A point, enter separator then continuously and separate and obtain the former powder of glyphosate.
When continuous crystallisation, crystalline particle is easy to precipitation and gathers the groove inner bottom part, for this reason, the present invention preferably is provided with circulating-pump outlet (being the C point) in the bottom of groove, make the in good time scour trough inner bottom part of recycle stock, prevents bigger crystal sedimentation, pyramidal structure is adopted in the bottom of crystallizer tank in addition, the crystalline particle of being convenient to precipitate is easier to be washed into awl by the charging of C point and to bring out mouth, suspends again, enters circulating system.
In addition; the B point can also be set on crystallizer among the present invention to link to each other with pump entry; and be provided with autocontrol valve; prevent when occurring unexpected; the D point stops up the back and produces negative pressure at the inlet of pump, makes pump generation cavitation, after negative pressure surpasses set(ting)value; B point automatic valve is opened, and guarantees that liquid circulation plays the effect of protection recycle pump.
Crystallizer tank described in the present invention can also be provided with a hot water inlet, as shown in the figure, is used for being used to scrub the recycle system when crystallization of washing possibility regularly takes place to stop up in the crystal of tube wall and in system.
The recycle system can adopt many recycle pumps among the present invention, and above-mentioned A point, B point, C point can be in all supporting uses of many recycle pumps, wherein B point and C point also can be only supporting use on the part recycle pump therein.
Crystallization time control temperature of charge is at 0-40 ℃ among the present invention, and mean residence time is 0.5-24 hour.With the hydrolyzed solution of alkyl esterification method production in adding alkali and after temperature of charge higher, be about more than 70 ℃, refrigerating unit crystallization control temperature can be set in the crystallisation cycle system.This refrigerating unit can be the built-in coil pipe of crystallizer tank, also can be placed on (as Fig. 1) on the circulation loop.
Alkali of the present invention comprises: ammonia, ammoniacal liquor, sodium hydroxide, potassium hydroxide etc. and their carbonate thereof.
Separator is continuous separator preferably, and can use many separators to separate continuously.
Method of the present invention can realize glyphosate serialization neutralization, crystallization, combine with other glyphosate serialization production workshop section effectively, realize the serialization of the whole process of glyphosate production, improve the stability and the level of automation of glyphosate production, make full use of the energy, reduce the glyphosate production cost.
Description of drawings
Fig. 1 is a continuous crystallisation process flow synoptic diagram.
Embodiment
The invention provides the method for continuous crystallisation in the glyphosate production, its process is as follows: during hydrolyzed solution enters continuously and the neutralization of still and liquid caustic soda, adjust pH value, in and still adopt the chuck cooling, the maintenance temperature is not higher than 90 ℃.In have a large amount of solids after becoming reconciled and separate out, adopt the solid-liquid transferpump that it is transported to the crystallization vat continuously, the crystallization that circulates, the crystallization vat adopts recycle system cooling, keeps 0 ~ 40 ℃ of temperature, ceaselessly carries separator to separate crystal solution simultaneously.
Embodiment 1
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 1.5, and mean residence time is 3h in the crystallization vat, and 20 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 2.0% after the filtration.
Embodiment 2
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 1.5, and mean residence time is 12h in the crystallization vat, and 20 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 1.9% after the filtration.
Embodiment 3
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 2, and mean residence time is 12h in the crystallization vat, and 30 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 1.8% after the filtration.
Embodiment 4
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 1.5, and mean residence time is 3h in the crystallization vat, and 30 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 2.3% after the filtration.
Embodiment 5
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 1.5, and mean residence time is 8h in the crystallization vat, and 20 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 1.7% after the filtration.
Embodiment 6
The hydrolyzed solution inlet amount is: 0.46 ton/h, adopting 32% liquid caustic soda to regulate pH value is about 2, and mean residence time is 8h in the crystallization vat, and 20 ℃ of Tcs are got mother liquor and measured the glyphosate content that does not crystallize out and get: 1.9% after the filtration.
Claims (3)
1. the method for the continuous crystallisation in the glyphosate production, wherein, the hydrolysate that is prepared in the glyphosate production by alkyl esterification method is continuously fed into and carries out crystallization in the circulation-type crystallizer after neutralization, the continuous discharging of the crystal solution of circulation advantages of good crystallization separates, it is characterized in that circulation-type crystallizer adopt recycle pump more than 2 to circulate and during crystallization the control temperature of charge at 0-40 ℃, mean residence time is 0.5-24 hour, the opening for feed of described recycle pump is connected with the conical lower portion of crystallisation vessel, described recycle pump has two outlets, is connected with the bottom with the middle part of crystallizer respectively.
2. method according to claim 1 is characterized in that described crystallizer middle part is provided with the B point and links to each other with the ingress of recycle pump.
3. method according to claim 2 is characterized in that described B point also is provided with by-pass valve control.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101761057A CN101423532B (en) | 2006-09-15 | 2006-09-15 | Continuous crystallisation process in glyphosate production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101761057A CN101423532B (en) | 2006-09-15 | 2006-09-15 | Continuous crystallisation process in glyphosate production |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610153244 Division CN1944445A (en) | 2006-09-15 | 2006-09-15 | Continuously crystallizing method in producing glyphosate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101423532A CN101423532A (en) | 2009-05-06 |
| CN101423532B true CN101423532B (en) | 2011-06-29 |
Family
ID=40614435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101761057A Active CN101423532B (en) | 2006-09-15 | 2006-09-15 | Continuous crystallisation process in glyphosate production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101423532B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1430622A (en) * | 2000-05-22 | 2003-07-16 | 孟山都技术有限责任公司 | Reaction systems for making N-(phosphonomethyl) glycine compounds |
-
2006
- 2006-09-15 CN CN2008101761057A patent/CN101423532B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1430622A (en) * | 2000-05-22 | 2003-07-16 | 孟山都技术有限责任公司 | Reaction systems for making N-(phosphonomethyl) glycine compounds |
Non-Patent Citations (1)
| Title |
|---|
| 陈晓祥等.烷基酯法生产草甘膦的技术进展.《现代化工》.1998,(第2期),第17-19页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101423532A (en) | 2009-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102432478B (en) | Preparation process of glycine | |
| CN101735270A (en) | Method for continuously crystallizing glyphosate | |
| CN112713269A (en) | Production system and production method for reducing content of sodium ions and sulfate ions in precursor of positive electrode material | |
| CN101736357B (en) | Method for continuous electrolytic synthesis of butanedioic acid | |
| CN101423532B (en) | Continuous crystallisation process in glyphosate production | |
| CN113750946B (en) | Reaction for preparing battery anode material precursor and purification system and process thereof | |
| CN1944445A (en) | Continuously crystallizing method in producing glyphosate | |
| CN207856912U (en) | A kind of lithium battery tertiary precursor synthesis apparatus system | |
| CN101445464A (en) | Method for preparing iminodiacetic acid from iminodiacetic acid disodium salt | |
| CN217051939U (en) | Sulfate radical desorption system in potash light brine | |
| CN105985251A (en) | Clean production process for amino acids such as iminodiacetic acid | |
| CN101139362A (en) | Continuous crystallization method for glyphosate production | |
| CN110723857B (en) | High-salinity water concentration and crystallization treatment system and process | |
| CN212293411U (en) | Mixed salt production system of sodium nitrate and potassium nitrate | |
| CN104945290B (en) | System for industrial preparation of 2-amino-5-naphtol7-sulfoacid | |
| CN217479356U (en) | Production device of dimethyl disulfide | |
| CN110787479A (en) | Purification and crystallization device for zinc sulfate production and preparation method thereof | |
| CN212403977U (en) | Calcium formate continuous production device | |
| CN217613020U (en) | Battery-grade lithium hydroxide continuous cooling crystallization system | |
| CN211078987U (en) | Device for producing urea phosphate by using wet-process phosphoric acid as raw material through elution crystallization | |
| CN210340945U (en) | Novel molasses dilution production line | |
| CN211078989U (en) | Device for producing urea phosphate by wet-process phosphoric acid elution coupling cooling crystallization | |
| CN216687516U (en) | Device system for producing potassium sulfate | |
| CN216023264U (en) | Nickel sulfate freezing crystallization device | |
| CN117018664A (en) | Lithium hydroxide freezing denitration crystallizer, purification system and purification method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |