CN107098813A - The preparation method and aldehyde-free colour stabilizer of DMAA - Google Patents
The preparation method and aldehyde-free colour stabilizer of DMAA Download PDFInfo
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- CN107098813A CN107098813A CN201710316552.7A CN201710316552A CN107098813A CN 107098813 A CN107098813 A CN 107098813A CN 201710316552 A CN201710316552 A CN 201710316552A CN 107098813 A CN107098813 A CN 107098813A
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- dmaa
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—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
- C07C209/08—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 amino groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
Chosen present invention relates particularly to the preparation method of the preparation method of DMAA and aldehyde-free colour stabilizer, wherein DMAA, including S1, raw material；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure；It is prepared by S2, crude product；Concentration is added to reactor for 25 40% dimethylamine, the temperature of reactor is controlled at 5 15 DEG C, chlorine propylene and liquid caustic soda are then added into reactor, stirring is warming up to 30 50 DEG C, reaction time was controlled at 48 hours, and cooling point liquid is that can obtain DMAA crude product after completion of the reaction；It is prepared by S3, sterling；DMAA crude product is distilled, 60 64 DEG C of cuts of collection are DMAA sterling.And aldehyde-free colour stabilizer DMAA as made from the above-mentioned preparation method referred to is formed with dimethyl diallyl ammonium chloride copolymerization.
Description
Technical field
The present invention relates to the preparation method of aldehyde-free colour stabilizer raw material, more particularly to the preparation method of DMAA and
Aldehyde-free colour stabilizer.
Background technology
In recent years with the development of water soluble polymer water purification agent and aldehyde-free colour stabilizer, both at home and abroad to the need of diallylamine
Ask and incrementally increase so that the relation between supply and demand of diallylamine changes, cause its price into the growth of geometry times.My company passes through
Cross research and find that DMAA is a kind of widely used organic compound, be mainly used in chemical intermediate, can conduct
Insecticide prepares the quaternary ammonium compound that auxiliary agent, additive are handled as various modified synthesis with other monomers copolymerization.
Especially its structure and the structure of diallylamine has similitude, with the monomer copolymerization such as dimethyl diallyl amine
The high molecular weight water soluble polymer of different purposes can be obtained.
The content of the invention
In view of the foregoing, it is an object to provide the new preparation method of DMAA and utilization should
Aldehyde-free colour stabilizer prepared by raw material.
The preparation method of DMAA, it is characterised in that
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 25-40% dimethylamine, the temperature of reactor is controlled at 5-15 DEG C,
Then chlorine propylene and liquid caustic soda are added into reactor, stirring is warming up to 30-50 DEG C, and the reaction time was controlled at 4-8 hours, had been reacted
Cooling point liquid is that can obtain DMAA crude product after finishing.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Further, in S2 steps, after reactor addition dimethylamine solution is finished, pass through chilled brine and control to react
Temperature in kettle is at 5-15 DEG C.
Further, in S2 steps, the feed postition of chlorine propylene and liquid caustic soda is using the two difference alternate dropwise addition.
Further, in S2 steps, the feed postition of chlorine propylene and liquid caustic soda is using dropwise addition simultaneously.
Further, in S2 steps, during chlorine propylene and liquid caustic soda dropwise addition, the temperature of control reactor is no more than 20
℃。
Further, in S2 steps, mixing speed control is controlled in 25-40min in 15-25r/min, mixing time.
Present invention also offers a kind of aldehyde-free colour stabilizer, its dimethyl-allyl as made from the above-mentioned preparation method referred to
Amine is formed with dimethyl diallyl ammonium chloride copolymerization.
Beneficial effects of the present invention are：
Prepared in the preparation method using chlorine propylene, dimethylamine, liquid caustic soda as raw material, its cost of material is compared to diallylamine
Prepare and have more the market competitiveness, at the same time, reactant in reactor is carried out using chilled brine in preparation process
The temperature control of system, will not produce other impurities, and chlorine propylene selects the mode being added dropwise to add to reactor with liquid caustic soda so that its
With dimethylamine during the course of the reaction more fully, and using the time of contact of each material in mixing control reaction system, accelerate anti-
The progress answered.
Embodiment
Preparation method and aldehyde-free colour stabilizer embodiment in conjunction with the embodiments to DMAA of the present invention is done further
Explanation.
Embodiment 1
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 25% dimethylamine, the temperature in reactor is controlled by chilled brine
Degree then adds chlorine propylene and liquid caustic soda, feed postition is using the two alternate dropwise addition, and being added dropwise respectively at 5 DEG C into reactor
Cheng Zhong, the temperature of control reactor is no more than 20 DEG C, stirs 25min, and mixing speed control 25r/min is warming up to 30 DEG C, reaction
Time control was at 4 hours, and cooling point liquid is that can obtain DMAA crude product after completion of the reaction.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Embodiment 2
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 40% dimethylamine, the temperature in reactor is controlled by chilled brine
Degree then adds chlorine propylene and liquid caustic soda, feed postition is using the two alternate dropwise addition, and being added dropwise respectively at 15 DEG C into reactor
Cheng Zhong, the temperature of control reactor is no more than 20 DEG C, stirs 40min, and mixing speed control 15r/min is warming up to 50 DEG C, reaction
Time control was at 8 hours, and cooling point liquid is that can obtain DMAA crude product after completion of the reaction.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Embodiment 3
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 33% dimethylamine, the temperature in reactor is controlled by chilled brine
Degree then adds chlorine propylene and liquid caustic soda, feed postition is using the two alternate dropwise addition, and being added dropwise respectively at 8 DEG C into reactor
Cheng Zhong, the temperature of control reactor is no more than 20 DEG C, stirs 27min, and mixing speed control 18r/min is warming up to 40 DEG C, reaction
Time control was at 6 hours, and cooling point liquid is that can obtain DMAA crude product after completion of the reaction.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Embodiment 4
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 33% dimethylamine, the temperature in reactor is controlled by chilled brine
Degree then adds chlorine propylene and liquid caustic soda, feed postition is using the two alternate dropwise addition, and being added dropwise respectively at 8 DEG C into reactor
Cheng Zhong, the temperature of control reactor is no more than 20 DEG C, stirs 30min, and mixing speed control 18r/min is warming up to 45 DEG C, reaction
Time control was at 6 hours, and cooling point liquid is that can obtain DMAA crude product after completion of the reaction.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Embodiment 5
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, bromopropene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 33% dimethylamine, the temperature in reactor is controlled by chilled brine
Degree then adds chlorine propylene, bromopropene and liquid caustic soda, feed postition is using dropwise addition, wherein chlorine third simultaneously at 8 DEG C into reactor
Dilute, bromopropene mass ratio control 1：During 1, and dropwise addition, the temperature of control reactor is no more than 20 DEG C, stirs 27min, stirring
Speed control 18r/min is warming up to 50 DEG C, and the reaction time was controlled at 6 hours, and cooling point liquid is that can obtain diformazan after completion of the reaction
Base allyl amine crude product.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
Embodiment 6
The preparation method of DMAA, including
S1, raw material are chosen；Dimethylamine, technical pure, bromopropene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 33% dimethylamine, the temperature in reactor is controlled by chilled brine
Spend at 8 DEG C, then addition bromopropene and liquid caustic soda into reactor, feed postition is used while during for dropwise addition, and dropwise addition, controlling
The temperature of reactor processed is no more than 20 DEG C, stirs 30min, and mixing speed control 18r/min is warming up to 45 DEG C, reaction time control
At 6 hours, cooling point liquid was that can obtain DMAA crude product after completion of the reaction.
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is dimethallyl
Base amine sterling.
DMAA sterling made from embodiment 1-6 and dimethyl diallyl ammonium chloride are subjected to copolymerization simultaneously
Reaction, obtains final cross-linking type aldehyde-free colour stabilizer.
The obtained DMAA of embodiment 1-4 and comparative example 1-3 is detected.Detect that data are as follows：
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although
The present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still can be right
Technical scheme described in foregoing embodiments is modified, or to which part technical characteristic carry out equivalent substitution, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc. should be included in the protection of the present invention
Within the scope of.
Claims (7)
1. the preparation method of DMAA, it is characterised in that
S1, raw material are chosen；Dimethylamine, technical pure, chlorine propylene, technical pure, liquid caustic soda, technical pure
It is prepared by S2, crude product；Concentration is added to reactor for 25-40% dimethylamine, the temperature of reactor is controlled at 5-15 DEG C,
Then chlorine propylene and liquid caustic soda are added into reactor, stirring is warming up to 30-50 DEG C, and the reaction time was controlled at 4-8 hours, had been reacted
Cooling point liquid is that can obtain DMAA crude product after finishing
It is prepared by S3, sterling；DMAA crude product is distilled, 60-64 DEG C of cut of collection is DMAA
Sterling.
2. the preparation method of DMAA according to claim 1, it is characterised in that in S2 steps, anti-
Answer kettle to add after dimethylamine solution finishes, the temperature in reactor is controlled at 5-15 DEG C by chilled brine.
3. the preparation method of DMAA according to claim 2, it is characterised in that in S2 steps, chlorine third
The feed postition of dilute and liquid caustic soda is using the two difference alternate dropwise addition.
4. the preparation method of DMAA according to claim 2, it is characterised in that in S2 steps, chlorine third
The feed postition of dilute and liquid caustic soda is using dropwise addition simultaneously.
5. the preparation method of DMAA according to claim 3, it is characterised in that in S2 steps, chlorine third
During dilute and liquid caustic soda is added dropwise, the temperature of control reactor is no more than 20 DEG C.
6. the preparation method of DMAA according to claim 5, it is characterised in that in S2 steps, stirring
Speed control is controlled in 25-40min in 15-25r/min, mixing time.
7. a kind of aldehyde-free colour stabilizer, it is characterised in that its dimethyl as made from the preparation method of any one of claim 1 to 6
Allyl amine is formed with dimethyl diallyl ammonium chloride copolymerization.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710316552.7A CN107098813A (en) | 2017-05-08 | 2017-05-08 | The preparation method and aldehyde-free colour stabilizer of DMAA |
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| CN201710316552.7A CN107098813A (en) | 2017-05-08 | 2017-05-08 | The preparation method and aldehyde-free colour stabilizer of DMAA |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4678474A (en) * | 1985-04-01 | 1987-07-07 | Nitto Boseki Co., Ltd | Method for improving color fastness of reactive dyes on cellulose with allylamine copolymer |
| CN102126965A (en) * | 2011-01-19 | 2011-07-20 | 中科院广州化学有限公司 | Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer |
| JP2014233706A (en) * | 2013-06-05 | 2014-12-15 | 三洋化成工業株式会社 | Organic coagulant |
-
2017
- 2017-05-08 CN CN201710316552.7A patent/CN107098813A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4678474A (en) * | 1985-04-01 | 1987-07-07 | Nitto Boseki Co., Ltd | Method for improving color fastness of reactive dyes on cellulose with allylamine copolymer |
| CN102126965A (en) * | 2011-01-19 | 2011-07-20 | 中科院广州化学有限公司 | Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer |
| JP2014233706A (en) * | 2013-06-05 | 2014-12-15 | 三洋化成工業株式会社 | Organic coagulant |
Non-Patent Citations (2)
| Title |
|---|
| 宫在礼: "活性染料耐氯固色剂的制备与应用", 《青岛大学硕士学位论文》 * |
| 杜杨等: "水溶性两性高分子的合成和溶液性质", 《精细化工》 * |
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