CN115784900A - Triethylamine purification method in glyphosate production process - Google Patents
Triethylamine purification method in glyphosate production process Download PDFInfo
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 title claims abstract description 401
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 47
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000000746 purification Methods 0.000 title claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 55
- 239000003463 adsorbent Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 claims abstract description 8
- 238000007670 refining Methods 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 239000003513 alkali Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 18
- 239000012452 mother liquor Substances 0.000 claims description 17
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000003795 desorption Methods 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000004471 Glycine Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
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- 239000007788 liquid Substances 0.000 description 10
- 150000001412 amines Chemical class 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 4
- 241000233948 Typha Species 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
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- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- -1 hetero amine Chemical class 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 240000000260 Typha latifolia Species 0.000 description 1
- 235000005324 Typha latifolia Nutrition 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
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- 238000012258 culturing Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- 230000008570 general process Effects 0.000 description 1
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- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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- 230000001502 supplementing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention discloses a triethylamine purification method in a glyphosate production process, wherein secondary triethylamine obtained through the steps of neutralization, layering, dehydration and the like is adsorbed, impurity components are removed through adsorption of an adsorbent to obtain refined triethylamine, the refined triethylamine is marked as tertiary triethylamine, and the refined triethylamine is stored in a triethylamine storage tank and is reused for synthesizing glyphosate; after a certain batch of secondary triethylamine is treated, hot water and steam are introduced into the adsorption tower to heat and desorb the adsorbent in a partition wall mode; after the adsorbent is desorbed, triethylamine is added again for secondary adsorption and refining. The invention effectively avoids the adverse effect of impurity component accumulation in the fraction on the glyphosate production.
Description
Technical Field
The invention belongs to the technical field of glyphosate by a glycine method, and particularly relates to a method for recovering and refining triethylamine.
Technical Field
The general process for producing glyphosate by the glycine method is as follows: in the synthesis process, formaldehyde, glycine and dimethyl phosphite are used as raw materials, methanol is used as a solvent, triethylamine is used as a catalyst, a synthetic solution is prepared, hydrochloric acid is added for acidolysis and hydrolysis reaction, the temperature is raised to remove the solvent, slurry containing glyphosate is obtained, glyphosate crystals are separated out by stirring, cooling and crystallizing and adding alkali to adjust the pH value in the crystallization process, then solid-liquid separation is carried out in the solid-liquid separation process, glyphosate wet powder and glyphosate acid mother liquor are obtained, and the glyphosate wet powder is dried to obtain a technical product. The glyphosate acid mother liquor is treated by adding liquid alkali to regenerate triethylamine, the triethylamine is separated into triethylamine at the upper layer (called neutralized triethylamine or primary triethylamine) and alkali mother liquor at the lower layer by standing and layering, the triethylamine at the upper layer is further dehydrated to obtain triethylamine (called dehydrated triethylamine or secondary triethylamine), the main content of the triethylamine can reach more than 99.0%, and the glyphosate removal synthesis process is used as a catalyst for recycling. Generally speaking, the triethylamine recovered by the method has high purity and lower single content of impurity components, is recycled for glyphosate production, and is basically not influenced particularly in the early production operation of a system, and the moisture index is generally mainly focused on technically. However, the research is further intensive, and the production performance is found to be reduced to some extent compared with the freshly supplemented triethylamine as the production time is prolonged, namely, the regeneration and recycling times of the triethylamine are increased. Analysis shows that the impurity amine (hybrid amine) enrichment problems such as monoethylamine, diethylamine, methylamine and the like exist, the production performance of glyphosate is influenced, and the phenomenon is of little concern. The hybrid amine is brought in by raw materials, products of triethylamine and glycine degradation and side reactions in the glyphosate production and mother liquor treatment processes are derived, and macromolecular amine substances such as aliphatic amine and the like and characteristic impurities such as isopropylamine and the like are also brought in some glyphosate production systems due to the production organization and process characteristics of the glyphosate production systems. Wherein, a small part of the hetero amine enters a water phase (alkali mother liquor) in the neutralization process, and because of the similarity and intermiscibility, a greater proportion of the hetero amine is enriched in the primary triethylamine and the secondary triethylamine, and cannot be effectively separated and discharged out of the system, and the enrichment effect is amplified along with the continuous accumulation and enrichment of the recycling of the triethylamine in a glyphosate production system and the prolonging of time until the quality of the triethylamine is serious and the energy efficiency and the conversion rate of the whole glyphosate production system are further influenced.
Production enterprises generally maintain the whole content level of the recovered triethylamine by a method of supplementing fresh triethylamine, but the method does not solve the problem from the source, only relieves the problem, and cannot radically cure the problem, and meanwhile, the unit consumption of the triethylamine is high. The method has the advantages that low-boiling hybrid amine in the triethylamine is removed by an enterprise through a method of rectifying secondary triethylamine regularly, but the method is high in energy consumption, high in safety risk, incomplete in removal of the low-boiling hybrid amine and ineffective in removal of macromolecular high-boiling hybrid amine, so that the method has limitations.
Disclosure of Invention
Aiming at the newly confirmed problems, the invention provides a process method for recovering and refining triethylamine, which is simple to operate, easy to transform and couple on the basis of the conventional process device for neutralizing and recovering triethylamine and low in operation energy consumption, and removes impurity components in the process of recovering triethylamine to obtain refined triethylamine (called tertiary triethylamine). The invention effectively avoids the adverse effect of impurity component accumulation in triethylamine on glyphosate production.
The triethylamine purification method in the glyphosate production process comprises the following steps:
s1, mixing acid mother liquor produced by glyphosate by a glycine method with alkali, reacting to regenerate triethylamine salt into triethylamine, standing and layering to obtain lower-layer alkali mother liquor and upper-layer triethylamine (namely neutralized triethylamine or primary triethylamine), and rectifying the lower-layer alkali mother liquor; the alkali is liquid alkali with the content of 30-52%, and the pH value range is controlled between 10-14;
s2, conveying the primary triethylamine in the step S1 to a dehydration kettle, adding alkali, stirring, dehydrating, and standing to obtain an upper layer triethylamine (called dehydrated triethylamine or secondary triethylamine) and a lower layer water phase (liquid alkali);
s3: and (3) conveying the secondary triethylamine in the step (S2) to an adsorption tower for refining, adsorbing by using a solid adsorbent to remove impurity components to obtain refined triethylamine (called as triethylamine after adsorption or tertiary triethylamine) with the content of more than 99.2%, and storing in a triethylamine storage tank for reuse in glyphosate synthesis.
S4: after a certain batch of secondary triethylamine is treated, hot water and steam are introduced into the adsorption tower to heat and desorb the adsorbent in a dividing wall mode, a fan is adopted to pump desorbed gas out of the adsorption tower, and the desorbed gas is treated by a tail gas removal device. Preferably, the desorption gas is subjected to condensation and absorption liquefaction.
S5: after the adsorbent is desorbed, triethylamine is added again for secondary adsorption and refining.
In step S3, the adsorption process is one-stage adsorption or multi-stage adsorption.
In the adsorption step, at least one stage of adsorbent is a solid adsorbent 1, and the adsorbent comprises the following raw materials in percentage by mass, wherein the total percentage by mass of the adsorbent is 100 percent: 80-100% of calcium chloride and 0-20% of active carbon. The adsorption process temperature is 15-60 ℃, preferably 20-42 ℃ from the comprehensive consideration of economy and effect; similar effects can also be obtained by partially or totally replacing the calcium chloride particles with magnesium chloride particles. The desorption temperature is 60-280 ℃, preferably 78-125 ℃, the desorption pressure is-101 KPa to +2KPa, and the desorption process is preferably in a micro negative pressure state.
Preferably, the adsorbent containing at least one stage of adsorption is a solid adsorbent 2, and the adsorbent comprises the following raw materials in percentage by mass, wherein the sum of the total mass percentages of the adsorbents is 100 percent: 60-100% of iron-rich biochar and 0-40% of filler, and the adsorption temperature is 10-80 ℃. The filler is ceramic particles or plastic particles.
The iron-rich biochar comes from a patent of preparation method and application of the iron-rich biochar of typha root, and the patent number is as follows: ZL 201910044643.9.
The invention has the beneficial effects that: according to the invention, the impurity components in the triethylamine are removed in the process of recycling the triethylamine to obtain the refined triethylamine, so that the adverse effect of accumulation of the impurity components in the triethylamine on glyphosate production is avoided. The method also has the advantages of simple operation, easy modification and coupling on the basis of the existing triethylamine neutralizing and recovering process device, and low operation energy consumption.
Drawings
FIG. 1 is a flow chart of a triethylamine purification method in the production process of glyphosate. 1. Triethylamine neutralizing mixer, 2 standing layering tank, 3 dehydrating kettle, 4 adsorbing tower, 5 desorbing tail gas processing device, 6 triethylamine storage tank, 7-1 transfer pump I, 7-2 transfer pump II and 7-3 blower.
Detailed Description
The above inventive process is further illustrated by the following specific examples:
example 1
Enumerating a device for implementing the invention, specifically a set of combination devices: the device specifically comprises a triethylamine neutralizing mixer, a standing layering tank, a dehydration kettle, an adsorption tower, a desorption tail gas treatment device and a triethylamine storage tank.
One end of the triethylamine neutralization mixer is connected with a liquid caustic soda and glyphosate acid mother liquor pipeline, and the other end of the triethylamine neutralization mixer is connected with the standing layering tank through a pipeline; the lower part of the standing layering tank is also connected with an alkali mother liquor discharge pipeline, and the middle upper part of the standing layering tank is connected with a dehydration kettle through a pipeline; the lower part of the dehydration kettle is also connected with a liquid caustic soda discharge pipeline, and the middle lower part of the dehydration kettle is provided with a triethylamine discharge port and a pipeline which are connected with one end of the adsorption tower through a transfer pump II; the other end of the adsorption tower is connected with a triethylamine storage tank through a pipeline; the triethylamine storage tank is connected with the glyphosate synthesizer through a pipeline.
The upper part of the adsorption tower is also provided with a desorption tail gas pipeline which is connected with a desorption tail gas treatment device; the desorption tail gas treatment device comprises a condensing device, an absorption device and a collecting tank;
the upper part and the lower part of the adsorption tower are respectively connected with a steam pipeline and a steam condensate water discharge pipeline;
the adsorption tower is a shell-and-tube tower, the adsorbent is filled in the tube, and the steam leaves the shell side.
Example 2
The apparatus of example 2, which is another example for implementing the present invention, is substantially the same as example 1, with the difference that: the adsorption tower is a packed tower, the adsorbent is filled in the tower, and a steam coil or a steam tube nest is arranged in the adsorption tower.
Example 3
Example 3 is substantially the same as example 2, listing another device for implementing the invention, except that: the device is also provided with a second-stage adsorption tower, the structure of the second-stage adsorption tower is similar to that of the first-stage adsorption tower, and the main difference lies in the difference of the adopted filler and the adopted adsorbent.
Example 4
Selecting an acid mother liquor of a system in which triethylamine is recycled for 120 times in a workshop production line (in the glyphosate production process, firstly, adding fresh triethylamine or recycled triethylamine which is added externally into a glyphosate synthesis reaction kettle to synthesize glyphosate, obtaining wet glyphosate powder and acid mother liquor after addition, condensation, hydrolysis, crystallization and solid-liquid separation, reacting the acid mother liquor with alkali to obtain primary triethylamine, dehydrating and drying to obtain secondary triethylamine, adding the secondary triethylamine as a raw material/catalyst into the synthesis reaction kettle to synthesize the next batch, sequentially adding, synthesizing, recycling triethylamine and feeding again to obtain a cycle), mixing the acid mother liquor and 30% liquid alkali in the process of producing glyphosate by a glycine method in a mixer, controlling the pH value between 13 and 14, regenerating triethylamine through neutralization and replacement reaction, standing and layering to obtain triethylamine (an upper layer) and an alkali mother liquor (a lower layer), conveying the triethylamine (a primary triethylamine) in the upper layer to the dehydration kettle, adding 98% of sheet alkali to dehydrate, recycling the dehydrated triethylamine (secondary triethylamine), wherein the main content is 99.3% and the water content is 0.18%. Conveying the secondary triethylamine to an adsorption tower for adsorption, and recovering to obtain the tertiary triethylamine, wherein the main content is 99.4 percent, and the water content is 0.16 percent. The adsorbent filled in the adsorption tower is as follows: 80% of calcium chloride particles and 20% of active carbon, and the adsorption temperature is controlled to be 20-30 ℃.
Example 5
Taking the primary triethylamine in the embodiment 4, collecting the primary triethylamine in a dehydration kettle, adding 98% caustic soda flakes for dehydration, and recovering to obtain secondary triethylamine, wherein the main content is 99.3% and the water content is 0.19%; and (3) conveying the secondary triethylamine to an adsorption tower for adsorption, and recovering to obtain tertiary triethylamine with the main content of 99.5% and the water content of 0.18%. The adsorbent filled in the adsorption tower is as follows: 98% of calcium chloride particles and 2% of active carbon, and the adsorption temperature is controlled to be 20-42 ℃.
Example 6
Taking the tertiary triethylamine obtained in the examples 4 and 5, and then passing through a packed column filled with an adsorbent 2, wherein the adsorbent filled in the packed column is iron-rich biochar prepared from iron-rich aquatic plants and part of PP ball filler (60% of the iron-rich biochar and 40% of the PP ball filler with the diameter of 8-20 mm). The triethylamine (quaternary triethylamine) after secondary adsorption is obtained, the main content is 99.65 percent, and the water content is 0.18 percent.
The preparation method of the iron-rich biochar prepared by the iron-rich aquatic plant comprises the following steps: (1) Selecting plants, cultivating and screening mature Typha latifolia which grows strongly, cleaning, putting into an incubator, self-cleaning in distilled water and Hoagland's nutrient solution for two-three weeks, adding FeSO4.7H2O solution, irrigating with FeSO4.7H2O solution at concentration of 0.1g/L, changing culture solution every week, and culturing for 2 months; (2) Preparation of cattail root-iron biochar comprises cutting plant parts of cattail with iron element, drying to no moisture, placing in a crucible, pumping air under closed condition, introducing nitrogen to balance pressure inside and outside the tube, adjusting nitrogen flow rate at 17mL/min, and sintering at 700 deg.C for 1h to obtain biochar; (3) And (3) ash removal treatment of the biochar, namely grinding the biochar, pouring 3mol/L NaOH solution into the grinded biochar, stirring the mixture at the temperature of 80 ℃ for 2 hours, filtering, washing with water, standing, pouring floating slag, and drying to obtain the iron-enriched biochar of the cattail roots.
Example 7
The secondary triethylamine obtained in the example 4, the secondary triethylamine obtained in the example 5, the tertiary triethylamine obtained in the example 4, the tertiary triethylamine obtained in the example 5 and the quaternary triethylamine obtained after the secondary adsorption obtained in the example 6 are respectively reused for synthesizing glyphosate, and the total yield of the glyphosate is respectively as follows: 84.8 percent, 83.7 percent, 85.6 percent, 85.7 percent and 86.6 percent, and the yield gradient relation is obvious.
Example 8
The device in the embodiment 1 is adopted to continuously operate according to the process scheme in the embodiment 4, when the recycled outlet triethylamine (tertiary triethylamine) is compared with the inlet triethylamine (secondary triethylamine) of the adsorption tower, the triethylamine content is kept level for 3 hours continuously, namely, the triethylamine content is not increased, the adsorption tower is judged to have no obvious refining effect, the adsorption tower is stopped, the liquid in the tower is drained from the lower part, a feeding valve of the triethylamine at the bottom and a discharging valve of the triethylamine at the top are closed, a tail gas desorption pipeline valve is opened, a shell-side steam valve and a condensate water drain valve of the adsorption tower are opened, the temperature at the top of the adsorption tower is controlled to be 100-110 ℃ by adjusting a steam valve, the micro negative pressure is controlled by a tail gas fan, the negative pressure suction and desorption are carried out for 200 minutes, and a small amount of nitrogen is supplemented from the bottom of the tower to drive the organic steam in the tower. After the desorbed gas is pumped out of the adsorption tower, the gas is condensed and absorbed for liquefaction and incineration treatment.
Claims (8)
1. A triethylamine purification method in the production process of glyphosate is characterized by comprising the following steps:
s1: mixing an acid mother liquor obtained by producing glyphosate by a glycine method with an alkali, reacting to regenerate triethylamine salt into triethylamine, standing and layering to obtain a lower-layer alkali mother liquor and an upper-layer triethylamine, and marking as primary triethylamine;
s2: conveying the primary triethylamine in the step S1 to a dehydration kettle, adding alkali, stirring, dehydrating, standing to obtain a lower-layer water phase and upper-layer triethylamine, and recording as secondary triethylamine;
s3: performing primary adsorption on the secondary triethylamine in the step S2, adsorbing by using an adsorbent to remove impurity components to obtain refined triethylamine, recording as tertiary triethylamine, storing in a triethylamine storage tank, and reusing in glyphosate synthesis;
s4: after a certain batch of secondary triethylamine is treated, hot water and steam are introduced into the adsorption tower to heat and desorb the adsorbent in a dividing wall mode, a fan is adopted to pump desorbed gas out of the adsorption tower, and the desorbed gas is treated by a tail gas removal device;
s5: and desorbing the adsorbent, and then adding triethylamine for the second time again for adsorption and refining.
2. The method for purifying triethylamine in the glyphosate production process according to claim 1, wherein the adsorption process in the step S3 is primary adsorption, the adsorbent is a solid adsorbent 1, and the sum of the solid adsorbent 1 in terms of the total mass percentage is 100%, and the method comprises the following raw materials in percentage by mass: 80-100% of calcium chloride and 0-20% of active carbon, and obtaining triethylamine for three times after adsorption.
3. The method for purifying triethylamine in the glyphosate production process according to claim 1, wherein the tertiary triethylamine obtained in the step S3 is subjected to secondary adsorption, and impurity components are removed through adsorption of an adsorbent to obtain refined triethylamine, namely the quaternary triethylamine, which is stored in a triethylamine storage tank and reused for synthesis of glyphosate.
4. The method for purifying triethylamine in the glyphosate production process according to claim 3, wherein the adsorbent for the secondary adsorption in step S3 is a solid adsorbent 2, and the solid adsorbent 2 comprises the following raw materials by weight percentage based on the total mass percentage of 100%: 60-100% of iron-rich biochar and 0-40% of filler, and obtaining triethylamine for four times after adsorption.
5. The method for purifying triethylamine in the glyphosate production process according to claim 4, wherein the primary adsorption temperature is 15-60 ℃.
6. The method for purifying triethylamine in the glyphosate production process according to claim 4, wherein the secondary adsorption temperature is 10-80 ℃.
7. The triethylamine purification method in the glyphosate production process according to claim 4, wherein the filler is ceramic particles or plastic particles.
8. The triethylamine purification method in the glyphosate production process according to claim 1, wherein the desorption temperature is 100-110 ℃ and the desorption pressure is-101 KPa to +2KPa.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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