A kind of benzalkonium chloride monomer synthesis technology
Technical field
The present invention relates to technology of fine chemicals, it is more particularly related to which a kind of benzalkonium chloride monomer closes
At technique.
Background technique
Benzalkonium chloride is a kind of cationic surfactant, also known as geramine, has wide spectrum, efficient sterilization algae removal energy
Power can efficiently control bacterium algae breeding and foundry loam growth in water, and have good sludge stripping effect and certain dispersion, seep
Effect thoroughly, at the same have it is certain deoil, deodorizing capability and corrosion inhibition, often do fungicide use in field of medicaments.
After the synthesis of benzalkonium chloride at present mostly uses dodecanol to synthesize dodecyl bromide, then react to obtain two with dimethylamine
Methyl dodecyl amine hydrogen bromide finally reacts to obtain benzalkonium chloride with benzyl chloride, and obtained benzalkonium chloride is mostly technical grade,
It is dfficult to apply to field of medicaments.Alkyl dimethylamine and benzyl chloride must be refined before the benzalkonium chloride preparation of pharmaceutical grade, the life
Production method process is complicated, and instrument and equipment requires height, and many medicinal benzalkonium chloride production companies can not prepare benzalkonium chloride,
Increase the cost of benzalkonium chloride medical product.
Summary of the invention
In order to solve above-mentioned technical problem in the prior art, the purpose of the present invention is to provide a kind of production cost is low
Benzalkonium chloride monomer synthesis technology.
In order to achieve the above-mentioned object of the invention, the invention adopts the following technical scheme:
A kind of benzalkonium chloride monomer synthesis technology, which comprises the steps of:
(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 is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills fatty alkyl dimethyl tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) the steam-heated heating device of starting TCU control, is warming up to 70-100 DEG C for reaction kettle, insulation reaction 7-
10 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and divides 2-5 cleaning crystal with ethyl acetate during filtering, and retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, after crystallization is complete, crystal is under the conditions of -1.5Mpa, 60 DEG C
Constant weight is dried under vacuum to up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Further, the molal weight of fatty alkyl dimethyl tertiary amine and benzyl chloride ratio is 1:1~1 in the step (1):
1.4。
Further, the fatty alkyl dimethyl tertiary amine in the step (1) is selected from Dodecyl Dimethyl Amine, 14
One of which in alkyl dimethyl tertiary amide, hexadecyldimethyl benzyl ammonium tertiary amine.
Further, in the step (2) additional amount of ethyl acetate fatty alkyl dimethyl tertiary amine can be completely dissolved
Subject to benzyl chloride.
Further, heating reaction unit described in the step (3) is the steam-heated collet of TCU control.
Further, in the step (5) ethyl acetate wash number in final crystal by fatty alkyl dimethyl uncle
Amine and benzyl chloride content are lower than subject to 0.005%.
Further, the additional amount of ethyl acetate is subject to and is completely dissolved filter cake in the step (6).
Further, the purity of acquired benzalkonium chloride monomer is greater than 99% in the step (6).
Compared with prior art, a kind of benzalkonium chloride monomer synthesis technology of the present invention has the advantages that.
For a kind of benzalkonium chloride monomer synthesis technology of the present invention compares traditional handicraft, benzalkonium chloride obtained is pure
Degree is high, impurity is few, and use is safe, can be effectively applied in field of medicaments.The present invention purifies benzene using the methods of recrystallization
Oronain is pricked, can be effectively reduced production cost, using the method energy that fatty alkyl dimethyl tertiary amine and benzyl chloride are added dropwise in proportion
Reaction efficiency and yield are enough improved, significant loss is avoided, further increases 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, it is tight raw material resources to be alleviated
, enrich the production ways of benzalkonium chloride.Benzalkonium chloride purity produced by the present invention is good, and precision is high, can by stable application in
Multiple fields.
Specific embodiment
A kind of benzalkonium chloride monomer synthesis technology of the present invention is done further below with reference to specific embodiment
It illustrates, to help those skilled in the art to have more complete, accurate and deep reason to inventive concept of the invention, technical solution
Solution.
Embodiment 1
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dimethyl are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills Dodecyl Dimethyl Amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 85 DEG C, insulation reaction 10 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 3 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 2
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl diformazan are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1.2;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills dodecyldimethylamine base tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 95 DEG C, insulation reaction 10 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 3 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 3
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the etradecyldimethylamine are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1.3;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 95 DEG C, insulation reaction 9 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 4 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 4
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dimethyl are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1.1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills Dodecyl Dimethyl Amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 85 DEG C, insulation reaction 9 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 3 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 5
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) Dodecyl Dimethyl Amine, benzyl chloride and ethyl acetate, the dimethyl are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, Dodecyl Dimethyl Amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills Dodecyl Dimethyl Amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 100 DEG C, insulation reaction 8 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 5 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 6
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl diformazan are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1.4;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills dodecyldimethylamine base tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 100 DEG C, insulation reaction 9 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 4 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 7
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) dodecyldimethylamine base tertiary amine, benzyl chloride and ethyl acetate, the fatty alkyl diformazan are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, dodecyldimethylamine base tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills dodecyldimethylamine base tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 80 DEG C, insulation reaction 9 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 2 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 8
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the etradecyldimethylamine are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 90 DEG C, insulation reaction 8.5 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 3 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Embodiment 9
A kind of benzalkonium chloride monomer synthesis technology, includes the following steps:
(1) hexadecyldimethyl benzyl ammonium tertiary amine, benzyl chloride and ethyl acetate, the etradecyldimethylamine are measured respectively by formula
The molal weight of base tertiary amine and benzyl chloride ratio is 1:1;
(2) ethyl acetate is put into 300L glassed steel reaction vessels, hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride is distinguished
It is pumped into head tank, the agitating device of reaction kettle is opened, instills hexadecyldimethyl benzyl ammonium tertiary amine and benzyl chloride in proportion under room temperature
In reaction kettle;
(3) heat riser is opened, reaction kettle is warming up to 95 DEG C, keeps the temperature anti-9.5 hours;
(4) recirculated cooling water is opened, product is cooled to room temperature, until crystal is precipitated completely;
(5) crystal being precipitated is taken out, decompression filters, and with 5 cleaning crystal of ethyl acetate point during filtering, retains filter
Cake;
(6) ethyl acetate is added in filter cake to be recrystallized, crystal is dried under vacuum under the conditions of -1.5Mpa, 60 DEG C
Constant weight is up to high-purity pharmaceutical grade benzalkonium chloride monomer.
Comparative example 1
Domiphen is squeezed into destilling tower, is distilled 30 hours under reduced pressure atmosphere, after distillation, leads to cool brine
Freezing 5 hours, and centrifugation is stirred, later by material by filtering kettle, room temperature filtering obtains material A;Benzyl chloride is pumped into steaming again
Tower is evaporated, is distilled 4 hours in the environment of 60 DEG C, obtains material B;Material A is pumped into reaction kettle, then material B is pumped into head tank,
It is heated while stirring in the environment of 56-60 DEG C and instills material B in reaction kettle, insulation reaction 2 hours, be then turned on circulation
Cooling water is cooled to room temperature to get product.
The performance difference for the benzalkonium chloride that embodiment 1-9 and comparative example 1 are prepared is as shown in table 1.
Table 1
。
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or not improved the conception and technical scheme of the invention are directly applied to other occasions
, it is within the scope of the present invention.