CN106946716A - A kind of benzalkonium chloride monomer synthesis technique - Google Patents
A kind of benzalkonium chloride monomer synthesis technique Download PDFInfo
- Publication number
- CN106946716A CN106946716A CN201710182322.6A CN201710182322A CN106946716A CN 106946716 A CN106946716 A CN 106946716A CN 201710182322 A CN201710182322 A CN 201710182322A CN 106946716 A CN106946716 A CN 106946716A
- Authority
- CN
- China
- Prior art keywords
- ethyl acetate
- tertiary amine
- benzalkonium chloride
- crystal
- synthesis technique
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to technology of fine chemicals, it is more particularly related to a kind of benzalkonium chloride monomer synthesis technique；Specifically include following steps：（1）Fatty alkyl dimethyl tertiary amine, benzyl chloride and ethyl acetate are measured respectively by formula；（2）By in ethyl acetate input Tang glass reaction kettle, fatty alkyl dimethyl tertiary amine and benzyl chloride are pumped into head tank respectively, opens and instills fatty alkyl dimethyl tertiary amine and benzyl chloride in reactor in proportion under the agitating device of reactor, normal temperature；（3）Reactor is warming up to 70 100 DEG C, insulation reaction 7 10 hours；（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；（5）The crystal separated out is taken out, suction filtration is depressurized, with 25 cleaning crystal of ethyl acetate point during filtering, retains filter cake；（6）Ethyl acetate is added in filter cake to be recrystallized, and after crystallization is complete, is drying to obtain.The production cost of the present invention is low, and obtained benzalkonium chloride purity is high.
Description
Technical field
The present invention relates to technology of fine chemicals, it is more particularly related to which a kind of benzalkonium chloride monomer is closed
Into technique.
Background technology
Benzalkonium chloride is a kind of cationic surfactant, also known as geramine, with wide spectrum, efficient sterilization algae removal energy
Power, can efficiently control bacterium algae in water and breed and foundry loam growth, and disperse, ooze with certain with good sludge stripping effect
Effect thoroughly, at the same have it is certain deoil, deodorizing capability and corrosion inhibition, often make bactericide in field of medicaments and use.
Synthesized more than the synthesis of current benzalkonium chloride using dodecanol after dodecyl bromide, then two are obtained with dimethylamine reaction
Methyl dodecyl amine hydrogen bromide, finally reacts to obtain benzalkonium chloride with benzyl chloride, and resulting benzalkonium chloride is mostly technical grade,
It is dfficult to apply to field of medicaments.The benzalkonium chloride of pharmaceutical grade must be refined alkyl dimethylamine and benzyl chloride before preparing, the life
Produce procedure complicated, instrument and equipment requires high, many medicinal benzalkonium chloride production companies can not prepare benzalkonium chloride,
Add the cost of benzalkonium chloride medical product.
The content of the invention
In order to solve above-mentioned technical problem of the prior art, it is an object of the invention to provide a kind of production cost is low
Benzalkonium chloride monomer synthesis technique.
In order to realize foregoing invention purpose, present invention employs following technical scheme：
A kind of benzalkonium chloride monomer synthesis technique, it is characterised in that comprise the following steps：
（1）Fatty alkyl dimethyl tertiary amine, benzyl chloride and ethyl acetate are measured respectively by formula；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, fatty alkyl dimethyl tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and fatty alkyl dimethyl tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Start the steam-heated heater of TCU controls, reactor is warming up to 70-100 DEG C, insulation reaction 7-10 is small
When；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 2-5 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Ethyl acetate is added in filter cake to be recrystallized, after crystallization is complete, crystal vacuum under the conditions of -1.5Mpa, 60 DEG C
Dry to constant weight and produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Further, the step（1）The molal weight ratio of middle fatty alkyl dimethyl tertiary amine and benzyl chloride is 1:1~1:
1.4。
Further, the step（1）In fatty alkyl dimethyl tertiary amine be selected from Dodecyl Dimethyl Amine, 14
One of which in alkyl dimethyl tertiary amide, hexadecyldimethyl benzyl ammonium tertiary amine.
Further, the step（2）The addition of middle ethyl acetate is can be completely dissolved fatty alkyl dimethyl tertiary amine
It is defined with benzyl chloride.
Further, the step（3）Described in heating response device be TCU control steam-heated chuck.
Further, the step（5）Middle ethyl acetate wash number with final crystal by fatty alkyl dimethyl uncle
Amine and benzyl chloride content are defined less than 0.005%.
Further, the step（6）The addition of middle ethyl acetate is defined so that filter cake is completely dissolved.
Further, the step（6）In obtained by the purity of benzalkonium chloride monomer be more than 99%.
Compared with prior art, a kind of benzalkonium chloride monomer synthesis technique of the present invention has the advantages that.
A kind of benzalkonium chloride monomer synthesis technique of the present invention is compared for traditional handicraft, and obtained benzalkonium chloride is pure
Degree is high, impurity is few, using safety, can be effectively applied in field of medicaments.The present invention purifies benzene using methods such as recrystallizations
Oronain is pricked, production cost can be effectively reduced, using the method energy that fatty alkyl dimethyl tertiary amine and benzyl chloride are added dropwise in proportion
Enough improve reaction efficiency and yield, it is to avoid significant loss, further improve product cost；In addition, the invention is adopted
Benzalkonium chloride is produced with dodecyldimethylamine base tertiary amine, hexadecyldimethyl benzyl ammonium tertiary amine are raw material, raw material resources can be alleviated tight
, enrich the production ways of benzalkonium chloride.Benzalkonium chloride purity produced by the present invention is good, high precision, can by stable application in
Multiple fields.
Embodiment
A kind of benzalkonium chloride monomer synthesis technique of the present invention is done further below with reference to specific embodiment
Illustrate there is more complete, accurate and deep reason to inventive concept of the invention, technical scheme to help those skilled in the art
Solution.
Embodiment 1
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dodecyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride are pumped into respectively
Head tank, opens and Dodecyl Dimethyl Amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 85 DEG C, insulation reaction 10 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 3 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 2
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1.2；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and dodecyldimethylamine base tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 95 DEG C, insulation reaction 10 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 3 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 3
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the hexadecyldimethyl benzyl ammonium uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1.3；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 95 DEG C, insulation reaction 9 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 4 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 4
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dodecyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1.1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride are pumped into respectively
Head tank, opens and Dodecyl Dimethyl Amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 85 DEG C, insulation reaction 9 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 3 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 5
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dodecyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride are pumped into respectively
Head tank, opens and Dodecyl Dimethyl Amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 100 DEG C, insulation reaction 8 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 5 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 6
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1.4；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and dodecyldimethylamine base tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 100 DEG C, insulation reaction 9 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 4 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 7
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl dimethyl uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and dodecyldimethylamine base tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 80 DEG C, insulation reaction 9 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 2 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 8
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the hexadecyldimethyl benzyl ammonium uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 90 DEG C, insulation reaction 8.5 hours；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 3 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 9
A kind of benzalkonium chloride monomer synthesis technique, comprises the following steps：
（1）Hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the hexadecyldimethyl benzyl ammonium uncle are measured respectively by formula
The molal weight ratio of amine and benzyl chloride is 1：1；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are pumped into respectively
Head tank, opens and hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride are instilled into reaction in proportion under the agitating device of reactor, normal temperature
In kettle；
（3）Heat riser is opened, reactor is warming up to 95 DEG C, anti-9.5 hours are incubated；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 5 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Add ethyl acetate in filter cake to be recrystallized, crystal is dried under vacuum to constant weight under the conditions of -1.5Mpa, 60 DEG C
Produce high-purity pharmaceutical grade benzalkonium chloride monomer.
Comparative example 1
Domiphen is squeezed into destilling tower, distilled 30 hours under reduced pressure atmosphere, after distillation is finished, leads to cool brine freezing
5 hours, and centrifugation is stirred, material is obtained into material A by filtering kettle, normal temperature filtering afterwards；Benzyl chloride is pumped into destilling tower again,
Distilled 4 hours in the environment of 60 DEG C, obtain material B；Material A is pumped into reactor, then material B is pumped into head tank, in 56-60
Heated while stirring in the environment of DEG C and instill material B in reactor, insulation reaction 2 hours is then turned on circulating cooling water-cooled
But to room temperature, product is produced.
The performance for the benzalkonium chloride that embodiment 1-9 and comparative example 1 are prepared is as shown in table 1 respectively.
Table 1
。
For the ordinary skill in the art, simply the present invention is exemplarily described for specific embodiment,
The obvious present invention, which is implemented, to be not subject to the restrictions described above, and is entered as long as employing method of the present invention design with technical scheme
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical scheme directly apply to other occasions
, within protection scope of the present invention.
Claims (8)
1. a kind of benzalkonium chloride monomer synthesis technique, it is characterised in that comprise the following steps：
（1）Fatty alkyl dimethyl tertiary amine, benzyl chloride and ethyl acetate are measured respectively by formula；
（2）Ethyl acetate is put into 300L glassed steel reaction vessels, fatty alkyl dimethyl tertiary amine and benzyl chloride are distinguished into pump
Enter head tank, open and instill fatty alkyl dimethyl tertiary amine and benzyl chloride instead in proportion under the agitating device of reactor, normal temperature
Answer in kettle；
（3）Start the steam-heated heater of TCU controls, reactor is warming up to 70-100 DEG C, insulation reaction 7-10 is small
When；
（4）ON cycle cooling water, room temperature is cooled to by product, is separated out completely to crystal；
（5）The crystal separated out is taken out, suction filtration is depressurized, with 2-5 cleaning crystal of ethyl acetate point during filtering, retains filter cake；
（6）Ethyl acetate is added in filter cake to be recrystallized, after crystallization is complete, crystal vacuum under the conditions of -1.5Mpa, 60 DEG C
Dry to constant weight and produce high-purity pharmaceutical grade benzalkonium chloride monomer.
2. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（1）Middle fatty alkyl
The molal weight ratio of dimethyl tertiary amine and benzyl chloride is 1:1~1:1.4.
3. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（1）In fatty alkane
Base dimethyl tertiary amine is in Dodecyl Dimethyl Amine, dodecyldimethylamine base tertiary amine, hexadecyldimethyl benzyl ammonium tertiary amine
One of which.
4. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（2）Middle ethyl acetate
Addition be defined so that fatty alkyl dimethyl tertiary amine and benzyl chloride can be completely dissolved.
5. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（3）Described in plus
Thermal reaction apparatus is the steam-heated chuck that TCU is controlled.
6. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（5）Middle ethyl acetate
Fatty alkyl dimethyl tertiary amine and benzyl chloride content are defined by wash number in final crystal less than 0.005%.
7. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（6）Middle ethyl acetate
Addition be defined so that filter cake is completely dissolved.
8. benzalkonium chloride monomer synthesis technique as claimed in claim 1, it is characterised in that the step（6）In obtained by benzene
The purity for pricking oronain monomer is more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710182322.6A CN106946716B (en) | 2017-03-24 | 2017-03-24 | Process for synthesizing benzalkonium chloride monomer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710182322.6A CN106946716B (en) | 2017-03-24 | 2017-03-24 | Process for synthesizing benzalkonium chloride monomer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106946716A true CN106946716A (en) | 2017-07-14 |
| CN106946716B CN106946716B (en) | 2019-03-01 |
Family
ID=59473437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710182322.6A Active CN106946716B (en) | 2017-03-24 | 2017-03-24 | Process for synthesizing benzalkonium chloride monomer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106946716B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553539A (en) * | 2017-09-27 | 2019-04-02 | 湖北葛店人福药用辅料有限责任公司 | A kind of preparation method of benzalkonium chloride |
| CN109553536A (en) * | 2017-09-27 | 2019-04-02 | 湖北葛店人福药用辅料有限责任公司 | A kind of synthetic method of fatty alkyl dimethylbenzyl based quaternary ammonium salt |
| CN113861037A (en) * | 2021-09-24 | 2021-12-31 | 泰柯棕化(张家港)有限公司 | Production process of low-residue medicinal benzalkonium chloride |
| CN115594593A (en) * | 2022-09-09 | 2023-01-13 | 四川博利恒药业有限公司（Cn） | Production process of benzalkonium chloride |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1287021A (en) * | 2000-07-05 | 2001-03-14 | 北京清华紫光英力化工技术有限责任公司 | Compound phase-transferring quaternary ammonium salt catalyst in beta-hydroxyl structure and its preparation |
| JP2002030044A (en) * | 2000-07-12 | 2002-01-29 | Sakai Chem Ind Co Ltd | Method for producing tetraalkylammonium halide |
| CN101050182A (en) * | 2006-04-06 | 2007-10-10 | 浙江华特实业集团华特化工有限公司 | Method for preparing quaternary ammonium salt |
| CN103351301A (en) * | 2013-07-01 | 2013-10-16 | 安徽奔马先端科技有限公司 | Synthetic method for high-purity quaternary ammonium salt |
| CN104163763A (en) * | 2014-07-14 | 2014-11-26 | 安徽奔马先端科技有限公司 | New synthesis method of high purity quaternary ammonium salt |
-
2017
- 2017-03-24 CN CN201710182322.6A patent/CN106946716B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1287021A (en) * | 2000-07-05 | 2001-03-14 | 北京清华紫光英力化工技术有限责任公司 | Compound phase-transferring quaternary ammonium salt catalyst in beta-hydroxyl structure and its preparation |
| JP2002030044A (en) * | 2000-07-12 | 2002-01-29 | Sakai Chem Ind Co Ltd | Method for producing tetraalkylammonium halide |
| CN101050182A (en) * | 2006-04-06 | 2007-10-10 | 浙江华特实业集团华特化工有限公司 | Method for preparing quaternary ammonium salt |
| CN103351301A (en) * | 2013-07-01 | 2013-10-16 | 安徽奔马先端科技有限公司 | Synthetic method for high-purity quaternary ammonium salt |
| CN104163763A (en) * | 2014-07-14 | 2014-11-26 | 安徽奔马先端科技有限公司 | New synthesis method of high purity quaternary ammonium salt |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553539A (en) * | 2017-09-27 | 2019-04-02 | 湖北葛店人福药用辅料有限责任公司 | A kind of preparation method of benzalkonium chloride |
| CN109553536A (en) * | 2017-09-27 | 2019-04-02 | 湖北葛店人福药用辅料有限责任公司 | A kind of synthetic method of fatty alkyl dimethylbenzyl based quaternary ammonium salt |
| CN109553539B (en) * | 2017-09-27 | 2022-05-03 | 湖北葛店人福药用辅料有限责任公司 | Preparation method of benzalkonium chloride |
| CN109553536B (en) * | 2017-09-27 | 2022-05-03 | 湖北葛店人福药用辅料有限责任公司 | Synthetic method of fatty alkyl dimethyl benzyl quaternary ammonium salt |
| CN113861037A (en) * | 2021-09-24 | 2021-12-31 | 泰柯棕化(张家港)有限公司 | Production process of low-residue medicinal benzalkonium chloride |
| CN115594593A (en) * | 2022-09-09 | 2023-01-13 | 四川博利恒药业有限公司（Cn） | Production process of benzalkonium chloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106946716B (en) | 2019-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106946716B (en) | Process for synthesizing benzalkonium chloride monomer | |
| JP2020045341A (en) | Continuous flow carboxylation reaction | |
| CN106631704A (en) | Preparation method for styrenated phenol | |
| CN106916068B (en) | Simple and convenient benzalkonium chloride production method | |
| CN107381589B (en) | Preparation method of ordered mesoporous silicon boron carbon nitrogen material | |
| CN106831446B (en) | Improved production method of pharmaceutical-grade benzalkonium chloride monomer | |
| CN103896781A (en) | Preparation method of benzyltriethylammonium chloride | |
| CN101643385A (en) | Method for preparing 3,5-dichlorobenzyl chloride | |
| CN104447303A (en) | Preparation technology of carboxybenzaldehyde | |
| CN109232508B (en) | Preparation method of 1, 1-cyclohexyl diacetic anhydride | |
| CN106187855B (en) | A method of 2- (hetero) aryl indole class compound is prepared using deep eutectic solvent | |
| CN102807494A (en) | Method for preparing fat alkyl dimethyl benzyl ammonium chloride | |
| CN105777802B (en) | A kind of process for purification of butyl titanate | |
| CN1919812A (en) | Refining method for hexafluoromethylene aromatic compound | |
| CN106946717A (en) | Benzalkonium chloride monomer synthesis technique | |
| CN102746238A (en) | Preparation method of pyrimethanil | |
| CN112010831A (en) | Green and efficient phenyl ether ketal bromination synthesis method | |
| CN106518687A (en) | Efficient preparation method of high-purity tetraethyl ammonium chloride | |
| CN104496892A (en) | Novel technology for synthesizing 4-dimethylamino-pyridine | |
| CN106674033A (en) | Preparation method of 2-aminoisobutyric acid | |
| CN107311843A (en) | A kind of 2,3 environmentally friendly dibromo Isosorbide-5-Nitrae butylene glycol preparation methods | |
| CN102464674B (en) | Preparation method of trichlorfon | |
| CN106905135A (en) | A kind of preparation method to bromomethyl phenylacetic acid | |
| CN110330443B (en) | Synthetic process of p-chlorophenylhydrazine hydrochloride | |
| CN107698503A (en) | A kind of preparation method of 8 fluorine quinoline and the preparation method of the fluorine quinoline of 3 iodine 8 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180706 Address after: 515000 block B, Chengde Square, Shantou Free Trade Zone, Shantou, Guangdong. Applicant after: Guangdong loest Pharmaceutical Co. Ltd. Address before: 515000 Shantou City, Guangdong province free trade zone Applicant before: Wu Lian |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 515000 one of the second floor of building 0001, block e08-4, Shantou Free Trade Zone, Shantou City, Guangdong Province Patentee after: Guangdong loest Pharmaceutical Co.,Ltd. Address before: 515000 block B, Chengde Square, Shantou Free Trade Zone, Shantou, Guangdong. Patentee before: Guangdong loest Pharmaceutical Co.,Ltd. |