CN117567307A - Neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride - Google Patents
Neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride Download PDFInfo
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- CN117567307A CN117567307A CN202311589884.4A CN202311589884A CN117567307A CN 117567307 A CN117567307 A CN 117567307A CN 202311589884 A CN202311589884 A CN 202311589884A CN 117567307 A CN117567307 A CN 117567307A
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- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 38
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 143
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 13
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- PHIQHXFUZVPYII-ZCFIWIBFSA-N (R)-carnitine Chemical compound C[N+](C)(C)C[C@H](O)CC([O-])=O PHIQHXFUZVPYII-ZCFIWIBFSA-N 0.000 description 11
- 239000006227 byproduct Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- JXXCENBLGFBQJM-UHFFFAOYSA-N (3-carboxy-2-hydroxypropyl)-trimethylazanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(O)CC(O)=O JXXCENBLGFBQJM-UHFFFAOYSA-N 0.000 description 3
- 229960001518 levocarnitine Drugs 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- BRLQWZUYTZBJKN-VKHMYHEASA-N (-)-Epichlorohydrin Chemical compound ClC[C@H]1CO1 BRLQWZUYTZBJKN-VKHMYHEASA-N 0.000 description 2
- GUYHPGUANSLONG-SNAWJCMRSA-N (E)-4-(trimethylammonio)but-2-enoate Chemical compound C[N+](C)(C)C\C=C\C([O-])=O GUYHPGUANSLONG-SNAWJCMRSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001212 derivatisation Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 210000001700 mitochondrial membrane Anatomy 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- BRLQWZUYTZBJKN-GSVOUGTGSA-N (+)-Epichlorohydrin Chemical compound ClC[C@@H]1CO1 BRLQWZUYTZBJKN-GSVOUGTGSA-N 0.000 description 1
- LHBPNZDUNCZWFL-SCSAIBSYSA-N (3r)-4-chloro-3-hydroxybutanenitrile Chemical compound ClC[C@H](O)CC#N LHBPNZDUNCZWFL-SCSAIBSYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 208000021642 Muscular disease Diseases 0.000 description 1
- 201000009623 Myopathy Diseases 0.000 description 1
- PUKNFWRLBQXPFL-FXRZFVDSSA-N [(e)-3-carboxyprop-2-enyl]-trimethylazanium;chloride Chemical compound [Cl-].C[N+](C)(C)C\C=C\C(O)=O PUKNFWRLBQXPFL-FXRZFVDSSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960004203 carnitine Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000007905 drug manufacturing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical group 0.000 description 1
- 150000002187 fatty acyl carnitines Chemical class 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 208000017169 kidney disease Diseases 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a neutralization and ammonium removal method of L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride, which comprises the following steps: step 1: transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle; step 2: introducing ammonium water into a neutralization and ammonium chloride removal reaction kettle; step 3: and (5) treating and neutralizing the materials in the ammonium chloride removal reaction kettle. The method reduces the impurity content and the dosage of ammonia water.
Description
Technical Field
The invention relates to a chemical method, in particular to a neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride.
Background
The L-carnitine can be used as a carrier to transport long-chain fatty acid from outside the mitochondrial membrane to inside the mitochondrial membrane in the form of fatty acyl carnitine, so that the oxidative decomposition of fatty acid is promoted, the endurance of human body is improved, and the fatigue feeling is reduced. It can also be used for treating nephropathy, lipid deposition myopathy, heart disease, etc. Thus, it is widely used.
The preparation method of L-carnitine comprises extraction, biosynthesis and chemical synthesis. The extraction method has low yield, more purification steps, high cost and difficult mass production. The biosynthesis method for preparing the L-carnitine mainly comprises two methods, namely a microbial fermentation method and enzymatic conversion. The chemical synthesis method mainly adopts two approaches: firstly, racemic carnitine is prepared, and a resolving agent is used for separating out a levorotatory body; and secondly, synthesizing by taking different chemical substances as raw materials. In the preparation of L-carnitine, L-3-carboxy-2-hydroxy-N, N, N-trimethylpropanammonium chloride is reacted with ammonium water to form an inner salt.
Chinese patent document CN101723843a discloses a method for preparing high purity levocarnitine. Belongs to the key technology of quality control of different links in the chiral drug production process. Detecting the content of the left-handed isomer impurity in the chiral raw material S-epichlorohydrin by gas chromatography and a chiral column, and controlling the content of the left-handed isomer impurity in the reaction raw material to be at a certain limit; detecting and controlling the specific rotation of the chiral intermediate L-3-chloro-2-hydroxypropyl trimethylammonium to a certain limit by using an optical rotation instrument; the method comprises the steps of detecting the content of a dextroisomer in an intermediate L-3-cyano-2-hydroxypropyl trimethylammonium by using a (+) alpha-methyl-6-methoxy-2-naphthalene acetyl chloride derivatization reagent in a combined way through an HPLC method, controlling the content of an optical isomer of the reaction intermediate to be a certain limit, and detecting a final product of levocarnitine by using the (+) alpha-methyl-6-methoxy-2-naphthalene acetyl chloride derivatization reagent in a combined way through the HPLC method. The detection and control method can obtain high-purity levocarnitine, wherein the content of the levorotatory isomer can reach more than 97%, and the content of the dextrorotatory isomer can reach less than 2%.
CN110372525a discloses a preparation method for synthesizing L-carnitine by taking R- (-) -epichlorohydrin as a starting material, which belongs to the field of pharmaceutical chemistry. The method comprises the following steps: firstly, R- (-) -epichlorohydrin and hydrocyanic acid are used as starting materials, and are reacted to synthesize R-4-chloro-3-hydroxybutyronitrile under the action of an alkaline catalyst; then the L-carnitine hydrochloride can be synthesized by two paths, and the final product L-carnitine is prepared after the L-carnitine hydrochloride prepared by the two paths is purified by resin to remove chloridion.
The neutralization and ammonium removal method in the prior art has low ammonium removal efficiency and inconvenient ammonium chloride recovery.
Disclosure of Invention
The invention provides a neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride aiming at the defects of the prior art.
The invention adopts the following scheme to realize the purposes:
the neutralization and ammonium removal method of the L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride comprises the following steps:
step 1: transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle;
step 2: introducing ammonium water into a neutralization and ammonium chloride removal reaction kettle;
step 3: and (5) treating and neutralizing the materials in the ammonium chloride removal reaction kettle.
Further, the mass fraction of the ammonium water introduced in the step 2 is 20%.
Further, in the step 2, ammonium water is introduced and the mixed solution is stirred.
Further, the ammonium water introduced in the step 2 is detected at the same time, and the introduction of the ammonium water is stopped when the pH value of the neutralization and ammonium chloride removal reaction kettle is 7-8.
Further, the temperature of the neutralization and ammonium chloride removal reaction kettle is controlled below 50 ℃ when ammonium water is introduced in the step 2.
Further, the step 3 is used for treating and neutralizing the materials in the ammonium chloride removal reaction kettle, and comprises the processes of negative pressure, heating and cooling.
The negative pressure is increased to the pressure of the neutralization and ammonium chloride removal reaction kettle to be stabilized at-0.08 MPa, and the temperature is increased to about 60-80 ℃; cooling to 25-35 ℃.
Further, after the material in the reaction kettle for neutralizing and removing ammonium chloride in the step 3 is finished, separating ammonium chloride by a centrifugal machine, and enabling the separated liquid to enter the next working procedure.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method has high neutralization and ammonium removal efficiency and reduces the consumption of ammonia water.
Detailed Description
In order to make the technical problems solved, the technical solutions adopted and the technical effects achieved by the present invention more clear, the technical solutions of the embodiments of the present invention will be described in further detail below, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The method of the invention is as follows:
transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle; introducing ammonium water into the neutralization and ammonium chloride removal reaction kettle, wherein the mass fraction of the introduced ammonium water is 20%, stirring the mixed solution while introducing the ammonium water, and stopping introducing the ammonium water when the pH value of the introduced ammonium water is 7-8; when the ammonium water is introduced, the temperature of the neutralization and ammonium chloride removal reaction kettle is controlled below 50 ℃; then, treating and neutralizing materials in the ammonium chloride removal reaction kettle, carrying out negative pressure and heating, and then cooling; the negative pressure is increased to the pressure of-0.08 MPa, the temperature is increased to 60-80 ℃, the solubility of ammonium chloride is gradually reduced along with the evaporation of water, and the ammonium chloride is gradually crystallized and separated out; the temperature is reduced to 25-35 ℃, the solubility of the ammonium chloride is further reduced along with the gradual reduction of the temperature, and part of the dissolved ammonium chloride is recrystallized and separated out. After the material in the reaction kettle for neutralizing and removing ammonium chloride is treated, separating ammonium chloride by a centrifugal machine, and taking the separated ammonium chloride as a byproduct for sale after barrelling, wherein the separated liquid enters the next working procedure.
The specific reaction principle of the process is as follows: the main reaction equation:
1: reacting hydrogen chloride with ammonium water to generate ammonium chloride:
HCl+NH 3 ·H 2 O→NH 4 Cl+H 2 O
2: the L-carnitine hydrochloride reacts with ammonium water to generate inner salt L-carnitine:
side reaction equation: the crotonobetaine hydrochloride reacts with ammonium water to produce crotonobetaine:
example 1
Transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle; introducing ammonium water into the neutralization and ammonium chloride removal reaction kettle, wherein the mass fraction of the introduced ammonium water is 20%, stirring the mixed solution while introducing the ammonium water, and stopping introducing the ammonium water when the pH value of the introduced ammonium water is 7-8; when the ammonium water is introduced, the temperature of the neutralization and ammonium chloride removal reaction kettle is controlled below 50 ℃; then, treating and neutralizing materials in the ammonium chloride removal reaction kettle, carrying out negative pressure and heating, and then cooling; the negative pressure is increased to the pressure of-0.08 MPa, the temperature is increased to 60-80 ℃, the solubility of ammonium chloride is gradually reduced along with the evaporation of water, and the ammonium chloride is gradually crystallized and separated out; the temperature is reduced to 25-35 ℃, the solubility of the ammonium chloride is further reduced along with the gradual reduction of the temperature, and part of the dissolved ammonium chloride is recrystallized and separated out. After the material in the reaction kettle for neutralizing and removing ammonium chloride is treated, separating ammonium chloride by a centrifugal machine, and taking the separated ammonium chloride as a byproduct for sale after barrelling, wherein the separated liquid enters the next working procedure.
Comparative example 1
Transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle; introducing ammonium water into the neutralization and ammonium chloride removal reaction kettle, wherein the mass fraction of the introduced ammonium water is 10%, stirring the mixed solution while introducing the ammonium water, and stopping introducing the ammonium water when the pH value of the introduced ammonium water is 7-8; and then treating materials in the neutralization and ammonium chloride removal reaction kettle, wherein the pressure of the neutralization and ammonium chloride removal reaction kettle is stabilized at 0.09MPa, the temperature is raised to about 90-95 ℃, the solubility of ammonium chloride is gradually reduced along with the evaporation of water, the ammonium chloride is gradually crystallized and separated out, meanwhile, the reaction kettle is naturally cooled, the solubility of ammonium chloride is further reduced along with the gradual reduction of temperature, and part of dissolved ammonium chloride is recrystallized and separated out. After the material in the reaction kettle for neutralizing and removing ammonium chloride is treated, separating ammonium chloride by a centrifugal machine, and taking the separated ammonium chloride as a byproduct for sale after barrelling, wherein the separated liquid enters the next working procedure.
Comparative example 2
Transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle; introducing ammonium water into the neutralization and ammonium chloride removal reaction kettle, wherein the mass fraction of the introduced ammonium water is 5%, stirring the mixed solution while introducing the ammonium water, and stopping introducing the ammonium water when the pH value of the introduced ammonium water is 7-8 and the pH value of the neutralization and ammonium chloride removal reaction kettle is detected; and then treating materials in the neutralization and ammonium chloride removal reaction kettle, wherein the pressure of the neutralization and ammonium chloride removal reaction kettle is normal pressure, the temperature is raised to about 98-100 ℃, the solubility of ammonium chloride is gradually reduced along with the evaporation of water, the ammonium chloride is gradually crystallized and separated out, and meanwhile, the reaction kettle is naturally cooled, the solubility of ammonium chloride is further reduced along with the gradual reduction of the temperature, and part of dissolved ammonium chloride is recrystallized and separated out. After the material in the reaction kettle for neutralizing and removing ammonium chloride is treated, separating ammonium chloride by a centrifugal machine, and taking the separated ammonium chloride as a byproduct for sale after barrelling, wherein the separated liquid enters the next working procedure.
The separation liquid in the above example was taken for analysis.
The invention effectively reduces the content of the crotonobetaine.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the technical principles of the present invention, and these modifications and variations should also be regarded as the scope of the invention.
Claims (8)
- The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride is characterized by comprising the following steps:step 1: transferring the mixed solution containing L-3-carboxyl-2-hydroxy-N, N, N-trimethyl ammonium chloride generated by hydrolyzing (L) -3-cyano-2-hydroxy propyl ammonium chloride into a neutralization and ammonium chloride removal reaction kettle;step 2: introducing ammonium water into a neutralization and ammonium chloride removal reaction kettle;step 3: and (5) treating and neutralizing the materials in the ammonium chloride removal reaction kettle.
- 2. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 1, characterized in that:and the mass fraction of the ammonium water introduced in the step 2 is 20%.
- 3. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 2, characterized in that:and (2) introducing ammonium water and stirring the mixed solution at the same time in the step (2).
- 4. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 1, characterized in that:and (3) simultaneously detecting the pH value of the neutralization and ammonium chloride removal reaction kettle by the ammonium water introduced in the step (2), and stopping introducing the ammonium water when the pH value is 7-8.
- 5. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 1, characterized in that:and (2) controlling the temperature of the neutralization and ammonium chloride removal reaction kettle to be below 50 ℃ when ammonium water is introduced in the step (2).
- 6. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 1, characterized in that:and 3, treating and neutralizing materials in the ammonium chloride removal reaction kettle in the step, wherein the process comprises the steps of negative pressure, heating and cooling.
- 7. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 1, characterized in that:the negative pressure is increased to the pressure of the neutralization and ammonium chloride removal reaction kettle to be stabilized at-0.08 MPa, and the temperature is increased to about 60-80 ℃; cooling to 25-35 ℃.
- 8. The neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethylpropylammonium chloride according to claim 7, characterized in that:and (3) separating ammonium chloride by a centrifugal machine after the material in the reaction kettle for neutralizing and removing ammonium chloride is finished in the step (3), and enabling the separated liquid to enter the next working procedure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311589884.4A CN117567307A (en) | 2023-11-27 | 2023-11-27 | Neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311589884.4A CN117567307A (en) | 2023-11-27 | 2023-11-27 | Neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride |
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| CN117567307A true CN117567307A (en) | 2024-02-20 |
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| CN202311589884.4A Pending CN117567307A (en) | 2023-11-27 | 2023-11-27 | Neutralization and ammonium removal method for L-3-carboxyl-2-hydroxy-N, N, N-trimethyl-propylammonium chloride |
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