CN105906804A - Production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride - Google Patents
Production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride Download PDFInfo
- Publication number
- CN105906804A CN105906804A CN201511012970.4A CN201511012970A CN105906804A CN 105906804 A CN105906804 A CN 105906804A CN 201511012970 A CN201511012970 A CN 201511012970A CN 105906804 A CN105906804 A CN 105906804A
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- CN
- China
- Prior art keywords
- poly
- production method
- hydroxypropyl
- dimethyl ammonium
- ammonium chlorides
- 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.)
- Pending
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 22
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims abstract description 14
- -1 hydroxypropyl Chemical group 0.000 claims description 51
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 10
- 150000007522 mineralic acids Chemical class 0.000 claims description 10
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 9
- 230000033228 biological regulation Effects 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 210000003298 dental enamel Anatomy 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 238000006068 polycondensation reaction Methods 0.000 claims description 4
- YWNYZQTZOONLGU-UHFFFAOYSA-N C(CC)Cl.[O] Chemical compound C(CC)Cl.[O] YWNYZQTZOONLGU-UHFFFAOYSA-N 0.000 claims 1
- 239000004593 Epoxy Substances 0.000 claims 1
- UPBLAVFWWWKVAJ-UHFFFAOYSA-N [Cl].CCC Chemical compound [Cl].CCC UPBLAVFWWWKVAJ-UHFFFAOYSA-N 0.000 claims 1
- 238000003756 stirring Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000012824 chemical production Methods 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 238000005189 flocculation Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000012643 polycondensation polymerization Methods 0.000 abstract 1
- 230000007423 decrease Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003974 emollient agent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/0206—Polyalkylene(poly)amines
- C08G73/0213—Preparatory process
- C08G73/0226—Quaternisation of polyalkylene(poly)amines
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical production and especially relates to a production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride. The production method comprises a, adding 33-34% of liquid dimethylamine with content of 35-42% and 33-34% of liquid epoxy chloropropane with content of 95-99% into a reactor and carrying out stirring through the reactor, b, carrying out condensation polymerization, c, carrying out gel chain reaction and d, adjusting a pH value. The product is transformed into a partial net structure from a linear structure, has a stable and firm structure and improves low viscosity, low molecular weight, a flocculation capability, water cleaning effects, temperature and salt resistance and a decomposition temperature to 250-350 DEG C.
Description
Technical field
Invention relates to chemical production technical field, relates to a kind of production method, refers in particular to a kind of poly-2 hydroxypropyls 1
The production method of 1 N alkyl dimethyl ammonium chloride.
Background technology
Poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides are applied in sewage disposal, mining and mineral process conduct
Cationic coagulant；It is used as aldehyde-free colour stabilizer in textile industry；In paper-making process, ripe as anion garbage capturing agent, AKD
Change accelerator；Acid fracturing cation modifier in oilfield applications is used as drilling clay stabilizer and water filling.Additionally, also
Emollient etc. as conditioning agent, antistatic additive, humidizer, shampoo and skin care.Visible it possesses goodish effect, but
The production efficiency being poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides is the highest, and yield rate is relatively low, and product
Improve purifying water effect, heatproof, the performance such as stable and do not reach the requirement that corresponding field needs.
Summary of the invention
The purpose of invention is for the problems referred to above, it is provided that a kind of production technology is simple, and yield rate is high, and structure is more stable and firm
Solid the production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides.
For reaching above-mentioned purpose, invent and have employed following technical proposal: poly-2 hydroxypropyl 11 N dimethyl
The production method of ammonium chloride, comprises the following steps: (a) add 33%-34% content be 35-42% liquid dimethyl amine and
33%-34% content is the liquid epoxy chloropropane of 95%-99%, adds reactor；It is stirred by reactor；B () is contracted
Poly-reaction；Temperature in reactor being controlled at 0-50 DEG C, Stress control carries out the reaction of 1-15 hour, (c) glue at 1-2mpa
Chain reaction；After front step program completes, then temperature being controlled at 80 95 DEG C, Stress control, at 2 5mpa, adds 33%-
34% auxiliary agent, described auxiliary agent includes dimethylamine, epoxychloropropane, ethylenediamine；And ratio is 1:1:0.02, carry out 35 hours
Reaction, reaction equation is as follows:
D () regulation pH value, in alkalescence in course of reaction, adds inorganic acid, making solution is neutrality；If PH is acidity, for making under PH
Fall can add alkali.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described step
Suddenly, in (d), described inorganic acid is Hcl or H2SO4 or acetic acid.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described step
Suddenly, in (d), described alkali is NaOH.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described is anti-
Still is answered to select enamel or stainless steel cauldron.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described is anti-
The paddle answering still uses paddle, speed of agitator 100 500 revs/min.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described step
Suddenly the addition in (d) regulation pH value is 0.1 0.5%.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described liquid
In state dimethylamine, methylamine content≤0.3 %, trimethylamine content≤0.5%；Ammonia content≤0.1%.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described liquid
The colourity of state epoxychloropropane :≤25；Relative density: 1.18 1.184；Moisture content≤0.5%.
In the production method of above-mentioned a kind of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, described second
The nonvolatile matter (%) of diamines: 0.06, fusing point (DEG C): 8 10 DEG C, boiling point (DEG C): 117 DEG C.
Compared with prior art, the advantage of invention is: obtains product by this method and is become part by linear structure
Network structure so that it is structure is more stable and firm, and low viscosity can improve its viscosity；Low-molecular-weight can improve its macromolecule
Amount；Flocculation ability strengthens, and improves purifying water effect；Improve heatproof, salt resistance ability；Improve its decomposition temperature (250 DEG C-350 DEG C).
Detailed description of the invention
Below in conjunction with using embodiment, the technical scheme in inventive embodiments is carried out clear, complete description, aobvious
So, described embodiment only invents a part of embodiment rather than whole embodiments.Based on the enforcement in invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into
The scope of invention protection.
Embodiment 1:
The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, comprises the following steps: (a) adds 35% and contain
The liquid epoxy chloropropane 34% of liquid dimethyl amine 33%, 95% content of amount, adds reactor；In liquid dimethyl amine, methylamine
Content=0.1 %, trimethylamine content=0.1%；Ammonia content=0.01%, the colourity of liquid epoxy chloropropane :=1；Relative density:
1.18；Moisture content=0.1%.
Reactor selects enamel or stainless steel cauldron, it is possible to while ensureing that reactor internal environment is stable, moreover it is possible to
Enough avoiding reactor itself to be etched, be stirred by reactor simultaneously, the paddle of reactor uses anchor formula or paddle, stirs
Mix rotating speed 100 revs/min, it is ensured that stir during reaction；(b) polycondensation reaction；Temperature in reactor is controlled at 0 DEG C, pressure
Control to carry out the reaction of 1 hour, (c) glue chain reaction at 1mpa；After front step program completes, then temperature is controlled at 80 DEG C, pressure
Power controls at 2mpa, adds 33% auxiliary agent, adds ethylenediamine, fusing point (DEG C): 8 DEG C, boiling point (DEG C): 117 DEG C, auxiliary agent includes diformazan
Amine, epoxychloropropane, ethylenediamine；And ratio is 1:1:0.02, reaction equation is as follows:
D () regulation pH value, in this step, addition is 0.1%.In alkalescence in course of reaction, addition inorganic acid, through upper reaction, makes
Solution is neutrality, and described inorganic acid is Hcl or H2SO4 or acetic acid；If PH is acidity, alkali can be added for making PH decline；Described
Alkali is NaOH.
Embodiment two:
The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, comprises the following steps: (a) adds 40% and contain
The liquid epoxy chloropropane 34% of liquid dimethyl amine 33%, 97% content of amount, adds reactor；In liquid dimethyl amine, methylamine
Content=0.2 %, trimethylamine content=0.3%；Ammonia content=0.05%, the colourity of liquid epoxy chloropropane :=15；Relative density:
1.182；Moisture content=0.3%.
Reactor selects enamel or stainless steel cauldron, it is possible to while ensureing that reactor internal environment is stable, moreover it is possible to
Enough avoiding reactor itself to be etched, be stirred by reactor simultaneously, the paddle of reactor uses anchor formula or paddle, stirs
Mix rotating speed 300 revs/min, it is ensured that stir during reaction；(b) polycondensation reaction；Temperature in reactor is controlled at 30 DEG C, pressure
Control to carry out the reaction of 10 hours, (c) glue chain reaction at 1.5mpa；After front step program completes, then temperature is controlled at 90 DEG C,
Stress control, at 4mpa, adds 33% auxiliary agent, adds ethylenediamine, fusing point (DEG C): 9 DEG C, boiling point (DEG C): 117 DEG C, auxiliary agent includes two
Methylamine, epoxychloropropane, ethylenediamine；And ratio is 1:1:0.02, reaction equation is as follows:
D () regulation pH value, in this step, addition is 0.3%.In alkalescence in course of reaction, addition inorganic acid, through upper reaction, makes
Solution is neutrality, and described inorganic acid is Hcl or H2SO4 or acetic acid；If PH is acidity, alkali can be added for making PH decline；Described
Alkali is NaOH.
Embodiment three
The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, comprises the following steps: (a) adds 42% and contain
The liquid epoxy chloropropane 33% of liquid dimethyl amine 33%, 99% content of amount, adds reactor；In liquid dimethyl amine, methylamine
Content=0.3 %, trimethylamine content=0.5%；Ammonia content=0.1%, the colourity of liquid epoxy chloropropane :=25；Relative density
1.184；Moisture content=0.5%.
Reactor selects enamel or stainless steel cauldron, it is possible to while ensureing that reactor internal environment is stable, moreover it is possible to
Enough avoiding reactor itself to be etched, be stirred by reactor simultaneously, the paddle of reactor uses anchor formula or paddle, stirs
Mix rotating speed 500 revs/min, it is ensured that stir during reaction；(b) polycondensation reaction；Temperature in reactor is controlled at 50 DEG C, pressure
Control to carry out the reaction of 15 hours, (c) glue chain reaction at 2mpa；After front step program completes, then temperature is controlled at 95 DEG C, pressure
Power controls at 5mpa, adds 34% auxiliary agent, adds ethylenediamine, fusing point (DEG C): 10 DEG C, boiling point (DEG C): 117 DEG C, auxiliary agent includes two
Methylamine, epoxychloropropane, ethylenediamine；And ratio is 1:1:0.02, reaction equation is as follows:
D () regulation pH value, in this step, addition is 0.5%.In alkalescence in course of reaction, addition inorganic acid, through upper reaction, makes
Solution is neutrality, and described inorganic acid is Hcl or H2SO4 or acetic acid；If PH is acidity, alkali can be added for making PH decline；Described
Alkali is NaOH.
The foregoing is only invention preferred embodiment, not in order to limit invention, all spirit in invention and principle
Within, any modification, equivalent substitution and improvement etc. done, within should be included in the protection domain of invention.
Claims (9)
- The production method of the most poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides, it is characterised in that comprise the following steps: A () adds the liquid dimethyl amine that 33%-34% content is 35-42% and the liquid ring that 33%-34% content is 95%-99% Oxygen chloropropane, adds reactor；It is stirred by reactor；(b) polycondensation reaction: the temperature in reactor is controlled at 0-50 DEG C, Stress control carries out the reaction of 1-15 hour at 1-2mpa, (c) glue chain reaction: after front step program completes, then by temperature control System is at 80 95 DEG C, and Stress control, at 2 5mpa, adds 33%-34% auxiliary agent, and described auxiliary agent includes dimethylamine, epoxy chlorine Propane, ethylenediamine, and ratio is 1:1:0.02, carries out the reaction of 35 hours, reaction equation is as follows:D () regulation pH value, in alkalescence in course of reaction, adds inorganic acid, making solution is neutrality；If PH is acidity, for making under PH Fall can add alkali.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levying and be, in described step (d), described inorganic acid is Hcl or H2SO4 or acetic acid.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levying and be, described alkali is NaOH.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levying and be, described reactor selects enamel or stainless steel cauldron.
- 5. according to the production method of the poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides described in claim 1 or 4, its Being characterised by, the paddle of described reactor uses paddle, speed of agitator 100 500 revs/min.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levy and be, described in step (d) regulation pH value addition is total amount 0.1 0.5%.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levy and be, in described liquid dimethyl amine, methylamine content≤0.3 %, trimethylamine content≤0.5%；Ammonia content≤0.1%.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levy and be, the colourity of described liquid epoxy chloropropane :≤25；Relative density: 1.18 1.184；Moisture content≤0.5%.
- The production method of poly-2 hydroxypropyl 11 N alkyl dimethyl ammonium chlorides the most according to claim 1, it is special Levy and be, the nonvolatile matter (%) of described ethylenediamine: 0.06, fusing point (DEG C): 8 10 DEG C, boiling point (DEG C): 117 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012970.4A CN105906804A (en) | 2015-12-31 | 2015-12-31 | Production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012970.4A CN105906804A (en) | 2015-12-31 | 2015-12-31 | Production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105906804A true CN105906804A (en) | 2016-08-31 |
Family
ID=56744331
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511012970.4A Pending CN105906804A (en) | 2015-12-31 | 2015-12-31 | Production method of poly-2-hydroxypropyl-1. 1-N-dimethyl ammonium chloride |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1003599A (en) * | 1973-07-19 | 1977-01-11 | Richard G. Tonkyn | Water-soluble cationic polymeric materials and their use |
| CN102153184A (en) * | 2011-05-11 | 2011-08-17 | 福州大学 | Composite organic and inorganic polymeric flocculant and preparation process and application of composite organic and inorganic polymeric flocculant |
| CN102198969A (en) * | 2010-03-22 | 2011-09-28 | 天津大港油田科远石油工程有限责任公司 | Oil-removing compound and its preparation method |
-
2015
- 2015-12-31 CN CN201511012970.4A patent/CN105906804A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1003599A (en) * | 1973-07-19 | 1977-01-11 | Richard G. Tonkyn | Water-soluble cationic polymeric materials and their use |
| CN102198969A (en) * | 2010-03-22 | 2011-09-28 | 天津大港油田科远石油工程有限责任公司 | Oil-removing compound and its preparation method |
| CN102153184A (en) * | 2011-05-11 | 2011-08-17 | 福州大学 | Composite organic and inorganic polymeric flocculant and preparation process and application of composite organic and inorganic polymeric flocculant |
Non-Patent Citations (3)
| Title |
|---|
| 金鹏等: "阳离子改性剂聚环氧氯丙烷-二甲胺的合成与应用", 《印染助剂》 * |
| 高宝玉等: "新型絮凝剂聚环氧氯丙烷胺的合成研究", 《环境化学》 * |
| 高宝玉等: "聚环氧氯丙烷胺的制备及其脱色性能", 《精细化工》 * |
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Application publication date: 20160831 |