CN114853614A - Triethylamine water removal device and water removal process - Google Patents
Triethylamine water removal device and water removal process Download PDFInfo
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- CN114853614A CN114853614A CN202210486298.6A CN202210486298A CN114853614A CN 114853614 A CN114853614 A CN 114853614A CN 202210486298 A CN202210486298 A CN 202210486298A CN 114853614 A CN114853614 A CN 114853614A
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- 238000000034 method Methods 0.000 title claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 42
- JEUXZUSUYIHGNL-UHFFFAOYSA-N n,n-diethylethanamine;hydrate Chemical compound O.CCN(CC)CC JEUXZUSUYIHGNL-UHFFFAOYSA-N 0.000 title claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 375
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 246
- 239000007788 liquid Substances 0.000 claims abstract description 102
- 230000005484 gravity Effects 0.000 claims abstract description 91
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 82
- 230000003068 static effect Effects 0.000 claims abstract description 68
- 239000003513 alkali Substances 0.000 claims abstract description 44
- 230000018044 dehydration Effects 0.000 claims abstract description 44
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 44
- 239000005562 Glyphosate Substances 0.000 claims abstract description 29
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229940097068 glyphosate Drugs 0.000 claims abstract description 29
- 238000002425 crystallisation Methods 0.000 claims abstract description 23
- 230000008025 crystallization Effects 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000004064 recycling Methods 0.000 claims abstract description 14
- 238000006386 neutralization reaction Methods 0.000 claims description 19
- 239000012452 mother liquor Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 101100356682 Caenorhabditis elegans rho-1 gene Proteins 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 239000010413 mother solution Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 1
- 238000004891 communication Methods 0.000 claims 1
- 239000011549 crystallization solution Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 18
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 11
- 238000004587 chromatography analysis Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WOAWYKPABZNBBV-UHFFFAOYSA-N 2-[bis(hydroxymethyl)amino]acetic acid Chemical compound OCN(CO)CC(O)=O WOAWYKPABZNBBV-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0237—Amines
- B01J31/0238—Amines with a primary amino group
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/3804—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)] not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
- C07F9/3813—N-Phosphonomethylglycine; Salts or complexes thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a triethylamine dewatering device and a process, wherein a crystallization liquid pipeline and a liquid caustic soda pipeline are respectively connected with a mixer, the mixer is connected with a first-stage gravity layer analyzer, the first-stage gravity layer analyzer is connected with a first-stage static distributor, the first-stage static distributor is connected with a second-stage gravity layer analyzer, the second-stage gravity layer analyzer is connected with a second-stage static distributor, the second-stage static distributor is connected with a dewatering kettle, and the dewatering kettle is connected with a static tank. The alkali separating tank is connected with a Y-shaped filter, and the Y-shaped filter is respectively connected with a liquid alkali pipeline and the elevated tank through pipelines by a material conveying pump; the elevated tank is respectively connected with the first-stage static distributor and the second-stage static distributor through pipelines. The problems that triethylamine is recycled in glyphosate production, the standing time is long, the moisture content is high, the yield of glyphosate products is influenced, the problem of recycling of alkali-separating concentrated alkali in a dehydration kettle is thoroughly solved, the liquid alkali of raw materials is reduced, the moisture brought by recycling triethylamine as the raw materials is reduced, the catalytic reaction rate is improved, and therefore the production cost of glyphosate of enterprises is reduced.
Description
Technical Field
The invention is designed and improved aiming at a device for recovering triethylamine moisture in glyphosate production, triethylamine is used as a catalyst in the glyphosate generation process, triethylamine hydrochloride is produced by hydrolysis under an acidic condition, and is neutralized with a sodium hydroxide solution to replace triethylamine, and the triethylamine is recycled to the glyphosate production for recycling. And static mixers are respectively added at outlets of two-stage layering grooves in a neutralization link, and the replaced triethylamine and the sodium hydroxide solution are mixed, so that free moisture in the triethylamine is further removed, and the purpose of quickly reducing the triethylamine moisture recovered in the glyphosate production is realized.
Technical Field
Glyphosate is currently the most widely used herbicide variety worldwide. Currently, the alkyl ester method is mainly adopted in China for production, methanol is used as a reaction solvent, glycine firstly reacts with paraformaldehyde to generate N, N-dimethylolglycine under the action of a catalyst triethylamine, then the N, N-dimethylolglycine reacts with dimethyl phosphite, and hydrochloric acid is added for hydrolysis to generate glyphosate. A large amount of triethylamine is needed as a catalyst in the production process, about 0.9t of triethylamine is needed for producing 1t of glyphosate raw medicine, the influence of the quality of triethylamine products on the yield of the glyphosate is large, and particularly, the control of triethylamine moisture indexes is very important for reducing the triethylamine moisture through one method.
The triethylamine continuous recovery process is that the filtered crystal liquid and sodium hydroxide solution with known mass fraction continuously enter a mixer according to a certain flow ratio (the flow of the crystal liquid is constant, and the flow of the sodium hydroxide is controlled according to the pH value) to carry out neutralization reaction, and the reaction heat is released. The solubility of triethylamine in the crystallization liquid is related to the temperature and is volatile, in order to control the temperature of the mixed liquid, the neutralized liquid discharged from a mixer directly enters a heat exchanger, enters a gravity layer separator for layering, the upper oil phase enters a triethylamine dehydration kettle, and is dehydrated by solid NaOH to obtain refined triethylamine, qualified triethylamine is obtained after fully standing in a small standing tank and a large standing tank for recycling, the standing time is 8-12h, and the water content of triethylamine can only be reduced to 0.3% from 0.8%. The lower water phase is filtered and then enters a recovery rectifying tower.
The invention reduces the water content of the recovered triethylamine, recycles the triethylamine to the synthesis procedure, recycles the triethylamine, and is important for stably controlling and improving the yield of the glyphosate.
Although the process method realizes the continuous recovery of triethylamine, the triethylamine used as a catalyst has long recycling standing time, high moisture, more production devices and large floor area, and is unfavorable for the positive direction of the glyphosate synthesis reaction. Meanwhile, solid NaOH is added into the dehydration kettle to absorb water, and then the solid NaOH is remained at the bottom of the dehydration kettle to form high-concentration caustic soda liquid, so that the solid NaOH is inconvenient to recycle. In conclusion, the water content of triethylamine is needed to be rapidly reduced by improving the recovery process.
Disclosure of Invention
Triethylamine is used as a catalyst, so that the conversion rate of the synthesis reaction is improved, the moisture in the triethylamine is reduced, and the turnover rate of the recovered triethylamine is improved, thereby improving the product yield. Static distributors are additionally arranged at outlets of the first-stage gravity chromatographic device and the second-stage chromatographic device, the upper oil phase is mixed with high-concentration liquid caustic soda, so that free water in the upper oil phase is adsorbed by the high-concentration liquid caustic soda, after two-stage adsorption, the water content of the recovered triethylamine can be reduced to be within 0.1% by adding solid NaOH in a dehydration kettle, and a solid foundation is provided for improving the yield of glyphosate products.
The invention utilizes the physical and chemical properties of triethylamine, is slightly soluble in water and has the relative density of 0.73g/cm 3 And (1) adding a static distributor at the outlets of the first-stage gravity layer analyzer and the second-stage gravity layer analyzer, and further removing free water in triethylamine from the upper oil phase triethylamine of the gravity layer analyzer and high-concentration liquid caustic soda through the static distributor. The high-concentration liquid caustic soda is obtained by adding flake caustic soda into a dehydration kettle and then absorbing water to dissolve the liquid caustic soda, the triethylamine on the upper part of the dehydration kettle is not discharged after discharging, a reflux pump is started to mix the high-concentration liquid caustic soda with a feeding material during feeding of the next batch, the mixture is kept stand for 15min before adding the flake caustic soda, the high-concentration liquid caustic soda is discharged from the bottom and is transferred to a roof elevated tank to be used in a static distributor to be mixed with the triethylamine, and the circulation is carried out in sequence. The specific technical scheme is as follows:
the utility model provides a triethylamine water trap, is specifically the apparatus for producing of retrieving triethylamine moisture in glyphosate production, and the crystallization liquid pipeline is connected with the blender respectively with the liquid alkali pipeline, and the blender is connected with one-level gravity chromatography ware, and one-level gravity chromatography ware is connected with one-level static distributor, and one-level static distributor is connected with second grade gravity chromatography ware, and second grade gravity chromatography ware is connected with second grade static distributor, and second grade static distributor is connected with the dehydration cauldron, and the dehydration cauldron is connected to the standing groove.
The dehydration kettle is also connected with an alkali separating tank; a pipeline from the dehydration kettle to the alkali separating tank is provided with an online monitoring proportion meter and a first valve; and a second valve is arranged on a pipeline from the dehydration kettle to the standing groove.
The alkali separating tank is connected with a Y-shaped filter, and the Y-shaped filter is respectively connected with a liquid alkali pipeline and the elevated tank through pipelines by a material conveying pump; and a third valve and a fourth valve are respectively arranged on the Y-shaped filter from the liquid caustic soda pipeline to the pipeline of the elevated tank.
The elevated tank is respectively connected with the primary static distributor and the secondary static distributor through pipelines;
and a fifth valve and a sixth valve are respectively arranged on the pipelines from the head tank to the first-stage static distributor and the second-stage static distributor.
The bottoms of the first-stage gravity layer analyzer and the second-stage gravity layer analyzer are connected to a rectification system through pipelines.
One-level gravity layer analyzer, second grade gravity layer analyzer are equal device, and gravity layer analyzer storage tank bottom is conical, is connected with U type return bend through the pipeline, and U type return bend top is connected with gravity layer analyzer top through gas phase balance pipe.
The middle part of the storage tank of the gravity layer analyzer is provided with a cross-shaped distributor, and the upper part of the storage tank is provided with an overflow pipe; the cross distributor and the U-shaped bent pipe realize the dewatering effect by controlling the height difference in the dewatering process; the height difference between the cross-shaped distributor and the overflow pipe is the height of triethylamine.
The cross distributor is provided with sieve pores with the pore diameter of phi 8-phi 12.
The structural design of the gravity chromatographic apparatus is characterized in that the U-shaped bend height is designed according to the neutralization flow of the crystallization liquid and the liquid alkali and the triethylamine content in the crystallization liquid, the residence time of triethylamine generated by reaction in the gravity chromatographic apparatus is controlled, and the longer the residence time is, the lower the water content is. The mixing effect is improved through the cross distributor inside, so that the light component triethylamine and the heavy component alkali crystallization liquid are effectively separated, and the light component triethylamine produced through reaction moves from the lower layer of the distributor to the upper layer, so that free water molecules in the triethylamine are separated, and the water content of the triethylamine is further reduced.
The invention also provides a production process for recovering triethylamine moisture in glyphosate production, which is carried out by adopting the device and comprises the following steps:
(1) adding the crystallization liquid and liquid caustic soda into a mixer for neutralization reaction, layering the reaction product by a gravity decanter and a static distributor in sequence after heat exchange, and feeding the separated upper oil phase into a dehydration kettle;
(2) starting stirring in a dehydration kettle, adding caustic soda flakes, continuously stirring until all the caustic soda flakes are melted, stopping stirring, standing, opening a first valve, and conveying the materials to an alkali separating tank; when the specific gravity count value of the materials from the dehydration kettle to the alkali separating tank is smaller than 1 by on-line monitoring, the first valve is automatically closed, and the second valve is opened to convey triethylamine to the standing tank for recycling.
(3) Alkali separation and recycling: and (3) when the content of the liquid caustic soda in the caustic soda separating tank is increased to 60-70%, adding a Y-shaped filter at the outlet of the caustic soda separating tank, adding a check valve at the outlet of the transfer pump, transferring the liquid caustic soda to a high-level tank through a valve, uniformly distributing the liquid caustic soda through a static distributor, then feeding the liquid caustic soda into a dehydration kettle, and performing the process step of the step (2) again to continuously obtain the triethylamine. And in the circulating process of continuously obtaining triethylamine, when the content of the liquid caustic soda transferred to the high-level tank is reduced to 40-45%, closing the third valve, opening the fourth valve, and transferring the low-concentration liquid caustic soda to a mixer for neutralizing with the crystallization liquid.
The pH value of the crystallization liquid in the step (1) is 1.0-1.5, the glyphosate is 1.2-2.0wt%, the triethylamine is 22-28 wt%, and the triethylamine exists in the form of hydrochloride;
the mass concentration of the liquid caustic soda is 38-42%, wherein the flow ratio of the liquid caustic soda to the crystallization liquid is 0.3-0.4;
after neutralization reaction, heat exchange is carried out to 40-50 ℃.
The gravity layer analyzer is a two-stage gravity layer analyzer, namely a first-stage gravity layer analyzer and a second-stage gravity layer analyzer; the static distributor is a two-stage static distributor, namely a first-stage static distributor and a second-stage static distributor.
The gravity decanter of the present invention: the layering plane is mainly controlled, the upper layer oil phase has higher water content if the layering plane is upward, and the lower layer water phase has increased triethylamine content if the layering plane is downward, which causes waste.
The gravity chromatographic apparatus is conical, the structural design key point is that the U-shaped bend height is designed according to the neutralization flow of the crystallization liquid and the liquid alkali and the triethylamine content in the crystallization liquid, the residence time of triethylamine generated by reaction in the gravity chromatographic apparatus is controlled, and the longer the residence time is, the lower the water content is. The mixing effect is improved through the cross distributor inside, so that the light component triethylamine and the heavy component alkali crystallization liquid are effectively separated, and the light component triethylamine produced through reaction moves from the lower layer of the distributor to the upper layer, so that free water molecules in the triethylamine are separated, and the water content of the triethylamine is further reduced.
The static distributor of the invention: the reaction temperature is mainly controlled to be not more than 55 ℃. The static distributor is a groove type distributor and is divided into an upper groove and a lower groove, so that an upper oil phase of a layering groove is fully mixed with high-concentration liquid caustic soda, and free water in triethylamine is taken away by combination of the high-concentration liquid caustic soda, so that the water content of the triethylamine is further reduced.
In the step (2), the adding mass ratio of the upper oil phase to the caustic soda flakes is 0.005-0.02; and standing for 20-30 minutes after stopping stirring.
The liquid caustic soda in the upper trough in the step (3) is divided into two branches which are respectively communicated with a first-stage static distributor and a second-stage static distributor for feeding;
opening a valve V, and separating an upper oil phase and liquid caustic soda flow through an outlet of the first-stage gravity layer separator according to a ratio of 1: (4-8) feeding to a primary static distributor;
after being uniformly mixed and distributed, the mixture enters a second-stage gravity layer analyzer, a valve VI is opened, and the flow of an upper-layer oil phase and the flow of a neutralization liquid alkali which are separated from an outlet of the second-stage gravity layer analyzer are as follows: (8-13) feeding to a secondary static distributor; and (3) uniformly mixing and distributing the mixture, then feeding the mixture into a dehydration kettle, and performing the process step of the step (2) again to obtain the triethylamine with low moisture content.
In the process of the invention, the height difference between the cross distributor 22 and the U-shaped bent pipe 21 in the first-stage gravity layer analyzer and the second-stage gravity layer analyzer is controlled to be H4,
h4 is disclosed as H2 ρ 1/ρ 2;
h2 is triethylamine height, H2 ═ H1 × V3/(V1+ V2);
H2-H4 is the amount of triethylamine in the upper layer, and the residence time of the triethylamine is controlled to be 20-30 minutes.
H1 is the total height of the material in the gravity decanter, H1 ═ V1+ V2)/S;
v1 represents the amount of the neutralized mother liquor (m) 3 )，V1＝V Mother liquor ；
V2 is the alkali content (m) of the neutralized liquid 3 )，V2＝K*V1；
V3 represents triethylamine (m) at the upper layer 3 )，V3＝V1*ρ3*m/ρ1；
V4 is lower mother liquor (m) 3 )，V4＝V1+V2-V3；
D is the inner diameter (m);
s is internal cross-sectional area (square meter), and pi D 2 /4；
Rho 1 is the specific gravity (g/ml) of the triethylamine in the upper layer;
ρ 2 is the specific gravity (g/ml) of the lower layer mother liquor;
rho 3 is the specific weight (g/ml) of the neutralization mother liquor;
k is the flow ratio of the liquid caustic soda to the mother liquor;
and M is the mass fraction of triethylamine in the mother solution.
The U-shaped bent height position is the layered surface position in the layered groove, and after the position of the cross distributor is determined, the height difference is increased to be the U-shaped bent height.
The inner diameter D of the present application can be set according to actual conditions on site.
The cross distributor is positioned, under the condition of determining the inner diameter, the triethylamine amount on the upper layer is determined according to actual feeding, the triethylamine amount on the upper layer is determined by subtracting the U-shaped bent height difference from the position H of the overflow port to the distributor, and the triethylamine amount on the upper layer can meet the condition that the triethylamine produced by reaction stays in the layered tank for no less than 0.5H.
And (3) uniformly mixing and distributing, then feeding into a dehydration kettle, and performing the process step of the step (2) again to obtain the triethylamine with low moisture content.
According to the technical scheme, when the dehydration kettle discharges the bottom before adding caustic soda flakes, in order to avoid discharging triethylamine into high-concentration liquid caustic soda, the dehydration kettle stops stirring to enable materials to fully stand, a specific gravity sensor is additionally arranged, and when the specific gravity is reduced, a bottom discharging valve is automatically closed. When the content of the concentrated alkali is reduced to 40% -45%, the part of the liquid alkali is recycled for neutralization and recovery of triethylamine, so that the consumption of the liquid alkali is saved.
After passing through a two-stage static distributor, the upper oil phase enters a dehydration kettle, after further dehydration is carried out through caustic soda flakes, the water content of the recovered triethylamine can be reduced to be below 0.12%, and the triethylamine can be reduced to be below 0.10% after standing for 4 hours in a later period through a standing tank.
The technical scheme of the invention is that a two-stage static distributor is added behind each stage of layering tank, high-concentration liquid caustic soda at the bottom of a dehydration kettle is recycled, free water molecules in the layering tank are fully adsorbed by virtue of large specific gravity difference and ion affinity, the concentration of the liquid caustic soda is gradually reduced along with continuous circulation, and the liquid caustic soda is transferred to a front-end triethylamine neutralization process for recycling when the concentration of the liquid caustic soda is lower than a certain value. The pH value of the crystallization liquid and the liquid caustic soda is mainly controlled through neutralization, the triethylamine is fully separated out through real-time adjustment of an online monitoring pH meter, an online monitoring specific gravity meter is added at the bottom of the dehydration kettle, and a bottom exhaust pneumatic valve is immediately closed when the specific gravity changes due to the fact that the specific gravity of the liquid caustic soda and the specific gravity of the triethylamine are greatly different, so that the triethylamine is prevented from being discharged into an alkali separating tank.
The water content has obvious influence on the yield of the glyphosate by consulting literature data, and references refer to the influence of the water content, the melting temperature and the hydrochloric acid content on the synthesis yield of the glyphosate, Lijunsheng, Gaoynpeng, pesticide, 2009, vol.48 and No. 8. See results and discussion.
The amount of triethylamine added in each batch of synthesis is about 2000kg, the water content is reduced by 0.2%, the water content in the raw materials is correspondingly reduced by 2000 x 0.2%, which is 4kg, and the total yield of the glyphosate is influenced by about 7%.
The 1% yield corresponds to an actual glyphosate yield of 12.06kg, and the yield of glyphosate can be increased by 0.01206 × 7 × 10000 ton to 882 ton, calculated as 1 ten thousand ton per month.
At present, the market price of glyphosate is 60000 ten thousand per ton, and the income can be increased by 5292 ten thousand yuan.
By adopting the technical scheme of the invention, the invention has the following beneficial effects: through install two-stage static distributor additional behind two-stage gravity chromatography ware, optimize operation process simultaneously, with high concentration liquid caustic soda circulation use, not only reduced liquid caustic soda consumption, more importantly through high concentration liquid caustic soda with the absorption of free hydrone in the triethylamine, reduced triethylamine moisture, improve synthetic reaction catalytic efficiency to improve the glyphosate yield, effectively reduced enterprise manufacturing cost. Meanwhile, the problems of long standing time for recycling triethylamine, large occupied area of production devices and the like are solved, the triethylamine turnover rate is increased, the storage capacity and the safety risk level of a production field are reduced, and the safety risk of an enterprise is effectively guaranteed.
Drawings
FIG. 1 shows a production apparatus for rapidly reducing the water content of triethylamine recovered in glyphosate production. 1. The system comprises a mixer, 2, a first-stage gravity layer analyzer, 3, a first-stage static distributor, 4, a second-stage gravity layer analyzer, 5, a second-stage static distributor, 6, a dehydration kettle, 7, an alkali separating tank, 8, a Y-shaped filter, 9, a head tank, 10, a crystallization liquid pipeline, 11, a liquid alkali pipeline, 12, an online monitoring hydrometer, 13, a valve I, 14, a valve II, 15, a valve III, 16, a valve IV, 17, a valve V, 18 and a valve VI.
FIG. 2 shows a gravity decanter unit wherein 19. piping for the crystallized liquid after neutralization, 20. blow-down pipe, 21. U-shaped pipe, 22. cross-shaped distributor, 23. overflow pipe, 24. vapor phase equilibrium pipe.
Fig. 3 shows a cross-shaped distributor, 25. mesh.
Detailed Description
Example 1
The utility model provides a reduce apparatus for producing of retrieving triethylamine moisture in glyphosate production fast, crystallization liquid pipeline 10 is connected with blender 1 respectively with liquid alkali pipeline 11, blender 1 is connected with one-level gravity chromatography ware 2, one-level gravity chromatography ware 2 is connected with one-level static distributor 3, one-level static distributor 3 is connected with second grade gravity chromatography ware 4, second grade gravity chromatography ware 4 is connected with second grade static distributor 5, second grade static distributor 5 is connected with dehydration cauldron 6, dehydration cauldron 6 is connected to the standing groove. The dehydration kettle 6 is connected with an alkali separating tank 7; a pipeline from the dehydration kettle 6 to the alkali separating tank 7 is provided with an online monitoring hydrometer 12 and a valve I13; and a second valve 14 is arranged on a pipeline from the dehydration kettle 6 to the standing groove.
The alkali separating tank 7 is connected with a Y-shaped filter 8, and the Y-shaped filter 8 is respectively connected with a liquid alkali pipeline 11 and a head tank 9 through pipelines by a feed delivery pump; and a third valve 15 and a fourth valve 16 are respectively arranged on the Y-shaped filter 8 from the liquid caustic soda pipeline 11 to the pipeline of the elevated tank 9. The elevated tank 9 is respectively connected with the primary static distributor 3 and the secondary static distributor 5 through pipelines; the pipelines from the head tank 9 to the first-stage static distributor 3 and the second-stage static distributor 5 are respectively provided with a valve five 17 and a valve six 18. The bottoms of the first-stage gravity layer analyzer 2 and the second-stage gravity layer analyzer 4 are connected to a rectification system through pipelines.
First order gravity layer analyzer 2, second grade gravity layer analyzer 4 are equal device, and gravity layer analyzer storage tank bottom is connected with U type return bend 21 through the pipeline, and U type return bend 21 top is connected with gravity layer analyzer top through gas phase balance pipe 24.
The middle part of the storage tank of the gravity layer analyzer is provided with a cross-shaped distributor 22, and the upper part is provided with an overflow pipe 23. The cross-shaped distributor 22 is provided with sieve pores 25, and the pore diameter of the sieve pores 25 is phi 8.
Example 2
Physical and chemical properties of the crystal liquid: acidity, pH value of 1.0-1.5, glyphosate content of about 1.5%, triethylamine content of about 25%, and water content of 1.2% (by mass, the triethylamine exists in the form of hydrochloride), and the triethylamine is a substance with high salt content, high total phosphorus content and high ammonia nitrogen content.
The process for recovering triethylamine moisture in the glyphosate production process by adopting the device in the embodiment 1 comprises the following steps:
(1) the content of liquid caustic soda is 40 percent, the flow ratio of the liquid caustic soda to the crystallization liquid is 0.4, the liquid caustic soda and the crystallization liquid are added into a mixer for neutralization reaction, the pH is controlled to be 10-10.8 by controlling the amount of the liquid caustic soda in the neutralization reaction process, the product after the reaction is subjected to heat exchange to 50 ℃, and then is sequentially layered by a first-stage gravity layer analyzer, a first-stage static distributor, a second-stage gravity layer analyzer and a second-stage static distributor, the reaction temperature is controlled by the static distributor, the temperature is not more than 55 ℃, and the separated upper oil phase enters a dehydration kettle;
(2) when the material is fed to the liquid level of 2/3 in the dehydration kettle, starting stirring, adding caustic soda flakes (0.025 x 2 ═ 0.05t), continuously stirring until the caustic soda flakes are completely melted, stopping stirring, standing for 30 minutes, starting a valve I, and sending the material to an alkali separating tank;
(3) alkali separation and recycling: when the content of liquid caustic soda in the caustic soda separating tank is increased to 70%, the outlet of the caustic soda separating tank is filtered by a Y-shaped filter, a check valve is added at the outlet of the transfer pump, and the liquid caustic soda is transferred to the high-level tank through a valve III and used for the static distributor.
(4) The static distributor controls the triethylamine moisture: two branches of liquid caustic soda in the upper trough in the step (3) are communicated with a first-stage static distributor and a second-stage static distributor for feeding, and a pneumatic regulating valve and a flowmeter are respectively added; the water content of triethylamine in the upper oil phase at the outlet of the layering tank of the first-stage gravity layer analyzer is about 0.8 percent, a valve V is opened, and the upper oil phase and the liquid caustic soda flow separated from the outlet of the first-stage gravity layer analyzer are in a proportion of 1: 5 (volume ratio) to a primary static distributor; after being uniformly mixed and distributed, the mixture enters a second-stage gravity layer analyzer, a valve VI is opened, and the flow of an upper-layer oil phase and the flow of a neutralization liquid alkali which are separated from an outlet of the second-stage gravity layer analyzer are as follows: 8 (volume ratio) to a secondary static distributor; and (3) uniformly mixing and distributing the mixture, then feeding the mixture into a dehydration kettle, and performing the process step in the step (2) again, wherein when the specific gravity count value of the material from the dehydration kettle to the alkali separating tank is monitored on line and is less than 1, the first valve is automatically closed, the second valve is opened to send triethylamine to the standing tank for recycling, so that triethylamine with low moisture content is obtained, circulation is realized, and along with continuous circulation, when the content of liquid alkali in the alkali separating tank in the step (3) is reduced to 40%, the third valve is closed, the fourth valve is opened, and the low-concentration liquid alkali is transferred to a mixer to be neutralized with the crystallization liquid for use.
The process selects the inner diameter of 1.8m and the inner cross section of 2.543m 2 4m of crystallization liquid 3 1.6m of liquid caustic soda with a content of 40% 3 In the second-stage gravity layer analyzer in the step (4), the triethylamine at the upper layer is 1.21m 3 The lower mother liquor is 4.39m 3 The total height is 2.2m, the height of triethylamine is calculated and controlled to be 0.48m, the height of mother liquor is 1.73m, and the height difference between the cross distributor and the U-shaped bent pipe is 0.29 m. When the specific gravity count value of the material from the dehydration kettle to the alkali separating tank is monitored on line and is less than 1, the first valve is automatically closed, the second valve is opened to send triethylamine to the standing tank for recycling, and the third valve is detectedThe water content of the ethylamine was 0.01%.
Aiming at the technical process, the height difference between the cross distributor with different inner diameters and regulation and control and the U-shaped bent pipe is also set, and the realized effect is as follows:
calculation of Triethylamine layered cell size
Calculation of height difference between triethylamine hierarchical groove cross distributor and U-shaped bend
Example 3
The steps of the method are the same as those of the embodiment 2, only the height difference between the cross-shaped distributor 22 and the U-shaped bent pipe 21 is controlled to be 0.29m, and after the circulation process is realized, the triethylamine in the step (2) is allowed to stand for 15min, so that the water content of the obtained triethylamine is 0.32%.
The steps of the method are the same as those of the embodiment 2, only the height difference between the cross-shaped distributor 22 and the U-shaped bent pipe 21 is controlled to be 0.29m, and after the circulation process is realized, the triethylamine in the step (2) is allowed to stand for 25min, so that the water content of the obtained triethylamine is 0.16%.
The steps of the method are the same as those of the embodiment 2, only the height difference between the cross-shaped distributor 22 and the U-shaped bent pipe 21 is controlled to be 0.29m, and after the circulation process is realized, the triethylamine is allowed to stand for 35min in the step (2), so that the water content of the obtained triethylamine is 0.07%.
The steps of the method are the same as those of the embodiment 2, only the height difference between the cross-shaped distributor 22 and the U-shaped bent pipe 21 is controlled to be 0.29m, and after the circulation process is realized, the triethylamine in the step (2) is allowed to stand for 40min, so that the water content of the obtained triethylamine is 0.06%.
Example 4
The steps of the method are the same as those of the embodiment 2, the adopted equipment of the embodiment 1 does not contain the U-shaped bent pipe 21, the control of the layering surface of the standing groove is not stable, the layering surface is too high, the moisture content of triethylamine is obviously increased, and the layering surface is too low, so that the triethylamine content in the mother solution at the lower layer of the layering groove is increased, and the recovery efficiency is influenced.
The steps of the method are the same as those of the example 2, only the adopted equipment of the example 1 does not contain the U-shaped bent pipe 21, the layering surface is 0.1m high, and after circulation is realized, the water content of the obtained triethylamine is 0.30%.
The steps of the method are the same as those of the embodiment 2, only the adopted equipment of the embodiment 1 does not contain the U-shaped bent pipe 21, the layering level is 0.2m, after circulation is realized, the water content of the obtained triethylamine is 0.44%, at the moment, part of the bottom mother liquor is carried into the triethylamine, and if the control is not carried out, the water content of the triethylamine can rise rapidly in the follow-up process.
Claims (10)
1. The utility model provides a triethylamine water trap, a serial communication port, crystallization liquid pipeline (10) and liquid caustic soda pipeline (11) are connected with blender (1) respectively, blender (1) is connected with one-level gravity layer analyzer (2), one-level gravity layer analyzer (2) are connected with one-level static distributor (3), one-level static distributor (3) are connected with second grade gravity layer analyzer (4), second grade gravity layer analyzer (4) are connected with second grade static distributor (5), second grade static distributor (5) are connected with dehydration cauldron (6), dehydration cauldron (6) are connected to the standing groove.
2. The triethylamine water removal device according to claim 1, wherein the dehydration kettle (6) is further connected with an alkali separation tank (7); a pipeline from the dehydration kettle (6) to the alkali separating tank (7) is provided with an on-line monitoring hydrometer (12) and a valve I (13); and a second valve (14) is arranged on a pipeline from the dehydration kettle (6) to the standing groove.
3. The triethylamine water removal device as claimed in claim 2, wherein the base separating tank (7) is connected with a Y-shaped filter (8), and the Y-shaped filter (8) is respectively connected with the liquid caustic soda pipeline (11) and the elevated tank (9) through pipelines by a material delivery pump; and a valve III (15) and a valve IV (16) are respectively arranged on the pipeline from the Y-shaped filter (8) to the liquid caustic soda pipeline (11) and the pipeline from the elevated tank (9).
4. The triethylamine water removal device according to claim 3, wherein the head tank (9) is connected with the primary static distributor (3) and the secondary static distributor (5) through pipelines respectively;
and the pipelines from the head tank (9) to the first-stage static distributor (3) and the second-stage static distributor (5) are respectively provided with a valve five (17) and a valve six (18).
5. The triethylamine water removal device according to claim 1, wherein the bottoms of the first-stage gravity layer analyzer (2) and the second-stage gravity layer analyzer (4) are connected to the rectification system through pipelines, the first-stage gravity layer analyzer (2) and the second-stage gravity layer analyzer (4) are identical devices, the bottom of the storage tank of the gravity layer analyzer is connected with the U-shaped bent pipe (21) through a pipeline, and the top of the U-shaped bent pipe (21) is connected with the top of the gravity layer analyzer through a gas phase balance pipe (24).
6. The triethylamine dewatering device according to claim 5, wherein a cross-shaped distributor (22) is disposed in the middle of the storage tank of the gravity layer analyzer, an overflow pipe (23) is disposed in the upper portion of the storage tank, a sieve mesh (25) is disposed on the cross-shaped distributor (22), and the diameter of the sieve mesh (25) is phi 8-phi 12.
7. The process for removing water by adopting the triethylamine water removing device as claimed in any one of claims 1 to 6,
the method comprises the following steps:
(1) adding the crystallization liquid and liquid caustic soda into a mixer for neutralization reaction, layering the reaction product by a gravity decanter and a static distributor in sequence after heat exchange, and feeding the separated upper oil phase into a dehydration kettle;
(2) starting stirring in a dehydration kettle, adding caustic soda flakes, continuously stirring until all the caustic soda flakes are melted, stopping stirring, standing, opening a first valve, and conveying the materials to an alkali separating tank;
(3) alkali separation and recycling: when the content of the liquid caustic soda in the caustic soda separating tank is increased to 60-70%, a Y-shaped filter is added at the outlet of the caustic soda separating tank, a check valve is added at the outlet of a transfer pump, the liquid caustic soda is transferred to a high-level tank through a valve III, the liquid caustic soda in the high-level tank is divided into two branches which are respectively communicated with a first-stage static distributor and a second-stage static distributor for feeding;
opening a valve V, and separating an upper oil phase and liquid caustic soda flow through an outlet of the first-stage gravity layer separator according to a ratio of 1: (4-8) feeding to a primary static distributor;
(4) after being uniformly mixed and distributed in the first-stage static distributor, the mixture enters a second-stage gravity layer separator, a valve VI is opened, and the flow of an upper oil phase and the flow of a neutralization liquid alkali which are separated from an outlet of the second-stage gravity layer separator are according to the ratio of 1: (8-13) feeding to a secondary static distributor;
and (3) uniformly mixing and distributing the mixture, then feeding the mixture into a dehydration kettle, and performing the process step of the step (2) again to obtain the triethylamine with low moisture content.
8. The process for removing water of claim 7, wherein the pH value of the crystallization solution in the step (1) is 1.0-1.5, the glyphosate is 1.2-2.0wt%, the triethylamine is 22-28 wt%, and the triethylamine is in the form of hydrochloride;
the mass concentration of the liquid caustic soda is 38-42%, wherein the flow ratio of the liquid caustic soda to the crystallization liquid is 0.3-0.4;
after neutralization reaction, heat exchange is carried out to 40-50 ℃.
9. The process for removing water according to claim 7, wherein the adding mass ratio of the upper oil phase to the caustic soda flakes in the step (2) is 0.005-0.02; standing for 20-30 minutes after stopping stirring; when the specific gravity counting value of the material from the dehydration kettle to the alkali separating tank is monitored on line and is less than 1, the first valve is automatically closed, and the second valve is opened to send triethylamine to the standing tank for recycling.
10. The process of claim 7, wherein the height difference between the cross-shaped distributor 22 and the U-bend 21 in the first stage gravity layer analyzer and the second stage gravity layer analyzer is H4,
h4 is disclosed as H2 ρ 1/ρ 2;
h2 is triethylamine height, H2= H1 × V3/(V1+ V2);
H2-H4 is the amount of triethylamine in the upper layer, and the residence time of the triethylamine is controlled to be 20-30 minutes;
h1 is the total height of the material in the gravity separator, H1= (V1+ V2)/S;
v1 for volume of neutralized mother liquor (mn), V1= V Mother liquor ；
V2 for medium alkali weight (mn), V2= K × V1;
v3, top triethylamine (mn), V3= V1 ρ 3 ρ 1;
v4 lower mother liquor (mn), V4= V1+ V2-V3;
d is the inner diameter (m);
s is the internal cross-sectional area (square meter), S = pi D 2 /4；
Rho 1 is the specific gravity (g/ml) of the triethylamine in the upper layer;
ρ 2 is the specific gravity (g/ml) of the lower layer mother liquor;
rho 3 is the specific weight (g/ml) of the neutralization mother liquor;
k is the flow ratio of the liquid caustic soda to the mother liquor;
and M is the mass fraction of triethylamine in the mother solution.
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