CN115746201B - Synthetic method of chlorine-free cationic rosin size emulsifier - Google Patents
Synthetic method of chlorine-free cationic rosin size emulsifier Download PDFInfo
- Publication number
- CN115746201B CN115746201B CN202211515273.0A CN202211515273A CN115746201B CN 115746201 B CN115746201 B CN 115746201B CN 202211515273 A CN202211515273 A CN 202211515273A CN 115746201 B CN115746201 B CN 115746201B
- Authority
- CN
- China
- Prior art keywords
- reaction
- rosin size
- chlorine
- parts
- size emulsifier
- 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.)
- Active
Links
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 30
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title claims abstract description 27
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title claims abstract description 27
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 25
- 238000010189 synthetic method Methods 0.000 title description 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 239000000178 monomer Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 11
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims abstract description 11
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001308 synthesis method Methods 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- 229910000856 hastalloy Inorganic materials 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 230000035484 reaction time Effects 0.000 abstract description 6
- RZWHKKIXMPLQEM-UHFFFAOYSA-N 1-chloropropan-1-ol Chemical compound CCC(O)Cl RZWHKKIXMPLQEM-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004945 emulsification Methods 0.000 abstract description 3
- 150000001768 cations Chemical class 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 16
- 238000006116 polymerization reaction Methods 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention provides a synthesis method of a chlorine-free cationic rosin size emulsifier, which comprises the following steps: mixing dimethyl diallyl ammonium chloride, acrylamide and dimethylaminoethyl methacrylate, and diluting with water to a certain concentration to obtain a mixed monomer solution; pumping the mixed monomer solution and the initiator into a micro-channel reactor from a raw material storage tank respectively through two metering delivery pumps for reaction at the reaction temperature of 60-100 ℃ and the pressure of 0.2-1.4 Mpa for reaction residence time of 0.5-3 min; transferring the materials into a cooling device for cooling treatment after the reaction to obtain the chlorine-free cation rosin size emulsifier. The invention solves the problems of high chloropropanol content and poor emulsification effect of the traditional rosin size emulsifier, and greatly shortens the reaction time by adopting a novel process of a microchannel reactor; greatly improves the conversion rate and the intrinsic viscosity of the product.
Description
Technical Field
The invention relates to the technical field of papermaking sizing agents, in particular to a method for synthesizing a cationic rosin size emulsifier.
Background
At present, most of cationic rosin size emulsifiers are epoxy polyamide resin emulsifiers or cationic emulsifiers prepared by copolymerization of various monomers and cationic monomers. There are many polymerization methods of chlorine-free cationic rosin size emulsifier, and the relatively mature synthesis method at home and abroad is to add initiator and metal ion chelating agent under nitrogen atmosphere and initiate copolymerization reaction of monomers at proper temperature. The method is intermittent reaction, the reaction materials in the reaction kettle have long reaction time, poor stirring and mixing effects and poor heat transfer effects, the reaction time is long, the conversion rate is low, the molecular weight distribution is uneven, the product quality is affected, the reaction control is difficult, the explosion polymerization can occur slightly carelessly, and the potential safety hazard exists.
Disclosure of Invention
The invention aims to solve the technical problems of high chloropropanol content and poor emulsification effect of the traditional rosin size emulsifier in the prior art, long polymerization reaction time in the synthesis of the emulsifier, uneven molecular weight, low conversion rate, easy explosion polymerization, potential safety hazard and the like.
The invention is realized by adopting the following technical scheme:
a synthesis method of a chlorine-free cationic rosin size emulsifier comprises the following steps:
S1, mixing dimethyl diallyl ammonium chloride, acrylamide and dimethylaminoethyl methacrylate, and diluting with water to a certain concentration to obtain a mixed monomer solution;
S2, pumping the mixed monomer solution and the initiator into a micro-channel reactor from a raw material storage tank respectively through two metering delivery pumps for reaction at the reaction temperature of 60-100 ℃ under the pressure of 0.2-1.4 Mpa for reaction residence time of 0.5-3 min;
and S3, transferring the materials to a cooling device for cooling treatment after the reaction to obtain the chlorine-free cationic rosin size emulsifier.
Preferably, the mass ratio of the mixed monomer to the initiator is 1:0.001-0.015.
Preferably, the initiator is at least one selected from ammonium persulfate, potassium persulfate, hydrogen peroxide, ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, hydrogen peroxide/tartaric acid, hydrogen peroxide/sodium metabisulfite, ammonium persulfate/ferrous sulfate, and hydrogen peroxide/ferrous sulfate.
Preferably, the mixed monomer comprises the following components in parts by weight: 15-30 parts of dimethyl diallyl ammonium chloride, 2-10 parts of acrylamide, 3-12 parts of dimethylaminoethyl methacrylate, and the content of the dimethyl diallyl ammonium chloride after being diluted by water is 30-80%.
Preferably, the material of the microchannel reactor is silicon carbide, stainless steel or hastelloy.
Preferably, the liquid holdup of the microchannel reactor is 20-1000mL.
The applicant has found that by adopting the specific monomer to carry out copolymerization reaction in a microchannel reactor, the chlorine-free cationic rosin size emulsifier with excellent characteristic viscosity and high conversion rate can be obtained unexpectedly, and the conversion rate can be up to more than 97%, which is far higher than that of a conventional kettle reactor. The applicant has completed the present invention based on the above findings.
The synthesis method of the chlorine-free cationic rosin size emulsifier solves the problems of high chloropropanol content and poor emulsification effect of the traditional rosin size emulsifier, replaces the traditional kettle type dripping process condition, and greatly shortens the reaction time by adopting a novel process of a microchannel reactor; the micro-channel reactor has extremely high heat and mass transfer efficiency, improves the reaction efficiency by means of the local vortex collision of fluid in the reactor, and greatly shortens the reaction time. The reaction temperature and the residence time can be accurately controlled by utilizing the microchannel reactor for reaction, and the continuous and safe production can be realized; the microchannel reactor reduces equipment requirements, is simple to operate, saves manpower, reduces occupied area and investment, and is suitable for industrial production.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and are not intended to limit the scope of the invention, as other obvious variations will occur to those skilled in the art. The basic principles of the invention defined in the following description may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
The apparatus or materials of the present invention are not identified to the manufacturer and are conventional commercial apparatus or materials. The detection indexes related to the embodiment of the invention are detected by adopting a conventional detection method in the field as not mentioned.
Example 1
A synthesis method of a chlorine-free cationic rosin size emulsifier comprises the following steps:
Step 1), adding water into 60 parts of monomer dimethyl diallyl ammonium chloride, 10 parts of acrylamide and 30 parts of dimethylaminoethyl methacrylate to dilute the mixture to 50%;
Step 2) pumping an ammonium persulfate aqueous solution and a monomer solution with the content of 50% into a micro-channel reactor from a raw material storage tank through two metering delivery pumps respectively, wherein the mass ratio of the ammonium persulfate to the monomer is 0.005:1, and the ammonium persulfate is diluted into a 5% aqueous solution by adding water;
Step 3) reacting in a microchannel reactor at a reaction temperature of 60 ℃ and a pressure of 0.2Mpa for a reaction residence time of 0.5min;
And 4) cooling the material after the reaction in the step 4) to obtain a polymer aqueous solution, namely the chlorine-free cationic rosin size emulsifier.
Wherein, the material of microchannel reactor is stainless steel, and the liquid holdup is 80mL.
Example 2
A synthesis method of a chlorine-free cationic rosin size emulsifier comprises the following steps:
step 1), 80 parts of monomer dimethyl diallyl ammonium chloride, 10 parts of acrylamide and 10 parts of dimethylaminoethyl methacrylate are diluted by water to 60 percent;
Step 2) respectively pumping the potassium persulfate/sodium bisulfate aqueous solution and the monomer with the content of 60% into a micro-channel reactor from a raw material storage tank through two metering delivery pumps, wherein the mass ratio of ammonium persulfate to the monomer is 0.015:1, and the potassium persulfate/sodium bisulfate aqueous solution is diluted into 5% aqueous solution by adding water;
Step 3) reacting in a micro-channel reactor at 100 ℃ under 0.5Mpa for 1min;
And 4) cooling the material after the reaction in the step 4) to obtain a polymer aqueous solution, namely the chlorine-free cationic rosin size emulsifier.
Wherein, the material of microchannel reactor is hastelloy, and the liquid holdup is 20mL.
Example 3
A synthesis method of a chlorine-free cationic rosin size emulsifier comprises the following steps:
Step 1), adding water into 60 parts of monomer dimethyl diallyl ammonium chloride, 30 parts of acrylamide and 10 parts of dimethylaminoethyl methacrylate to dilute to 40%;
Step 2) pumping the potassium persulfate aqueous solution and the monomer with the content of 40% into a microchannel reactor from a raw material storage tank through two metering delivery pumps respectively, wherein the mass ratio of the potassium persulfate to the monomer is 0.01:1, and the potassium persulfate is diluted into 5% aqueous solution by adding water;
step 3) reacting in a micro-channel reactor at 90 ℃ under 0.8Mpa for 2min;
And 4) cooling the material after the reaction in the step 4) to obtain a polymer aqueous solution, namely the chlorine-free cationic rosin size emulsifier.
Wherein the micro-channel reactor is made of silicon carbide, and the liquid holdup is 200mL.
Example 4
The synthesis method of the chlorine-free cationic rosin size emulsifier comprises the following steps:
step 1) adding water into 80 parts of monomer dimethyl diallyl ammonium chloride, 20 parts of acrylamide and 20 parts of dimethylaminoethyl methacrylate to dilute to 70%;
step 2) pumping the potassium persulfate aqueous solution and the monomer with the content of 70% into a microchannel reactor from a raw material storage tank through two metering delivery pumps respectively, wherein the mass ratio of hydrogen peroxide to the monomer is 0.015:1, and the hydrogen peroxide is diluted into 5% aqueous solution by adding water;
step 3) reacting in a micro-channel reactor at 80 ℃ under 1.4Mpa for 3min;
And 4) cooling the material after the reaction in the step 4) to obtain a polymer aqueous solution, namely the chlorine-free cationic rosin size emulsifier.
Wherein the micro-channel reactor is made of silicon carbide, and the liquid holdup is 200mL.
Comparative example:
A synthesis method of a chlorine-free cationic rosin size emulsifier comprises the following steps:
Placing the monomer aqueous solution into a four-neck flask with a thermometer, adding EDTA (accounting for the mass of the monomer aqueous solution) with the mass fraction of 0.007%, a proper amount of Ammonium Persulfate (APS) solution and deionized water, regulating 60 parts of dimethyl diallyl ammonium chloride, 30 parts of acrylamide and 10 parts of dimethylaminoethyl methacrylate, uniformly stirring, introducing nitrogen into a reaction system to deoxidize for about 20min, controlling the temperature of 40 ℃ (feeding temperature) of the reaction system, uniformly mixing the system, heating the system by sections to respectively reach the polymerization initiation temperature of 46 ℃, the polymerization reaction temperature of 50 ℃ and the polymerization reaction curing temperature of 70 ℃, and cooling and discharging after each section is reacted for 3 h.
The intrinsic viscosity and monomer conversion of the product polymers of each example and comparative example were determined.
Performance test experiment:
characteristic viscosity: the characteristic viscosity eta of the product is measured in a water bath at 30 ℃ by using a Ubbelohde viscometer with 1mol/L sodium chloride aqueous solution as a solvent.
Conversion rate: the solid content and the monomer conversion rate of the product are measured according to a GB/T12005.2-1989 polyacrylamide solid content measuring method and a GB/T22312-2008 plastic polyacrylamide residual acrylamide content measuring method. The detection results are shown in Table 1.
TABLE 1 conversion and product intrinsic viscosity for different preparation methods
| Sample of | Conversion/% | Value of intrinsic viscosity eta |
| Example 1 | 97.3 | 1.78 |
| Example 2 | 98.5 | 1.86 |
| Example 3 | 98.4 | 1.86 |
| Example 4 | 97.7 | 1.77 |
| Comparative example | 87.6 | 1.13 |
The detection effect proves that the chlorine-free cationic rosin size emulsifier prepared by the method has extremely high conversion rate, and the characteristic viscosity of the product is superior to that of the product prepared by the conventional method, so that the molecular weight distribution is more uniform, the operation is simple and easy to control.
It will be appreciated by persons skilled in the art that the above embodiments are by way of example only and not limiting of the invention. The objects of the present invention have been fully and effectively achieved. The functional and structural principles of the present invention have been shown and described in the examples and embodiments of the invention may be modified or practiced without departing from the principles described.
Claims (6)
1. The synthesis method of the chlorine-free cationic rosin size emulsifier is characterized by comprising the following steps of:
S1, mixing dimethyl diallyl ammonium chloride, acrylamide and dimethylaminoethyl methacrylate, and diluting with water to a certain concentration to obtain a mixed monomer solution, wherein the mixed monomer comprises the following components in parts by weight: 15-30 parts of dimethyl diallyl ammonium chloride, 2-10 parts of acrylamide and 3-12 parts of dimethylaminoethyl methacrylate;
S2, pumping the mixed monomer solution and the initiator into a micro-channel reactor from a raw material storage tank respectively through two metering delivery pumps for reaction at the reaction temperature of 60-100 ℃ under the pressure of 0.2-1.4 Mpa for reaction residence time of 0.5-3 min;
and S3, transferring the materials to a cooling device for cooling treatment after the reaction to obtain the chlorine-free cationic rosin size emulsifier.
2. The method of claim 1, wherein the mass ratio of the mixed monomer to the initiator is 1:0.001-0.015.
3. The method of claim 1, wherein the initiator is selected from at least one of ammonium persulfate, potassium persulfate, hydrogen peroxide, ammonium persulfate/sodium bisulfite, potassium persulfate/sodium bisulfite, hydrogen peroxide/tartaric acid, hydrogen peroxide/sodium metablock, ammonium persulfate/ferrous sulfate, hydrogen peroxide/ferrous sulfate.
4. The method of claim 1, wherein the microchannel reactor is made of silicon carbide, stainless steel, or hastelloy.
5. The method of claim 1, wherein the microchannel reactor has a liquid holdup of from 20 mL to 1000mL.
6. A chloride-free cationic rosin size emulsifier prepared according to the method of any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211515273.0A CN115746201B (en) | 2022-11-30 | 2022-11-30 | Synthetic method of chlorine-free cationic rosin size emulsifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211515273.0A CN115746201B (en) | 2022-11-30 | 2022-11-30 | Synthetic method of chlorine-free cationic rosin size emulsifier |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115746201A CN115746201A (en) | 2023-03-07 |
| CN115746201B true CN115746201B (en) | 2024-05-10 |
Family
ID=85340890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211515273.0A Active CN115746201B (en) | 2022-11-30 | 2022-11-30 | Synthetic method of chlorine-free cationic rosin size emulsifier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115746201B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1073591A (en) * | 1996-08-30 | 1998-03-17 | Technol Res Assoc Of Medical & Welfare Apparatus | Micro flow passage element |
| CN105111366A (en) * | 2015-07-08 | 2015-12-02 | 杭州市化工研究院有限公司 | Aqueous solution polymerization preparation method of methacrylamidopropyltrimethylammonium chloride and acrylamide copolymer |
| CN106279533A (en) * | 2016-08-29 | 2017-01-04 | 上海东升新材料有限公司 | A kind of cationic rosin size emulsifying agent and preparation method thereof |
| CN106660006A (en) * | 2014-07-02 | 2017-05-10 | 康宁股份有限公司 | Synthesis of an acrylic polymer in flow reactor |
| CN107236133A (en) * | 2016-03-29 | 2017-10-10 | 上海东升新材料有限公司 | A kind of preparation method of cationic rosin size |
| CN108396589A (en) * | 2018-02-06 | 2018-08-14 | 齐鲁工业大学 | A kind of cationic rosin size emulsifier and preparation method thereof |
| CN110407973A (en) * | 2018-04-27 | 2019-11-05 | 上海东升新材料有限公司 | A kind of preparation method of gum rosin cationic emulsifier |
| CN111171368A (en) * | 2020-01-20 | 2020-05-19 | 杨恺 | Preparation method and device of UV-cured environment-friendly thermal expansibility microsphere |
| CN111978461A (en) * | 2020-08-31 | 2020-11-24 | 滁州金桥德克新材料有限公司无锡分公司 | Water-based functional acrylic resin and preparation method thereof |
| CN113150204A (en) * | 2021-03-15 | 2021-07-23 | 浙江大学衢州研究院 | Method for preparing soap-free acrylic polymer material by microchannel continuous flow active polymerization |
| CN113845617A (en) * | 2021-11-30 | 2021-12-28 | 江苏富淼科技股份有限公司 | Method for continuously preparing polyacrylamide inverse emulsion |
| CN114573755A (en) * | 2022-05-05 | 2022-06-03 | 山东奥赛新材料有限公司 | Preparation method of cationic emulsifier for rosin size |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3003572B1 (en) * | 2013-03-25 | 2015-03-27 | Seppic Sa | NOVEL AMPHIPHILIC POLYMERS AND THEIR USE IN THE TREATMENT OF SURFACES OF HYDROPHOBIC MATERIALS |
| EP3250614A1 (en) * | 2015-01-30 | 2017-12-06 | Basf Se | Reverse-phase polymerisation process incorporating a microfluidic device |
-
2022
- 2022-11-30 CN CN202211515273.0A patent/CN115746201B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1073591A (en) * | 1996-08-30 | 1998-03-17 | Technol Res Assoc Of Medical & Welfare Apparatus | Micro flow passage element |
| CN106660006A (en) * | 2014-07-02 | 2017-05-10 | 康宁股份有限公司 | Synthesis of an acrylic polymer in flow reactor |
| CN105111366A (en) * | 2015-07-08 | 2015-12-02 | 杭州市化工研究院有限公司 | Aqueous solution polymerization preparation method of methacrylamidopropyltrimethylammonium chloride and acrylamide copolymer |
| CN107236133A (en) * | 2016-03-29 | 2017-10-10 | 上海东升新材料有限公司 | A kind of preparation method of cationic rosin size |
| CN106279533A (en) * | 2016-08-29 | 2017-01-04 | 上海东升新材料有限公司 | A kind of cationic rosin size emulsifying agent and preparation method thereof |
| CN108396589A (en) * | 2018-02-06 | 2018-08-14 | 齐鲁工业大学 | A kind of cationic rosin size emulsifier and preparation method thereof |
| CN110407973A (en) * | 2018-04-27 | 2019-11-05 | 上海东升新材料有限公司 | A kind of preparation method of gum rosin cationic emulsifier |
| CN111171368A (en) * | 2020-01-20 | 2020-05-19 | 杨恺 | Preparation method and device of UV-cured environment-friendly thermal expansibility microsphere |
| CN111978461A (en) * | 2020-08-31 | 2020-11-24 | 滁州金桥德克新材料有限公司无锡分公司 | Water-based functional acrylic resin and preparation method thereof |
| CN113150204A (en) * | 2021-03-15 | 2021-07-23 | 浙江大学衢州研究院 | Method for preparing soap-free acrylic polymer material by microchannel continuous flow active polymerization |
| CN113845617A (en) * | 2021-11-30 | 2021-12-28 | 江苏富淼科技股份有限公司 | Method for continuously preparing polyacrylamide inverse emulsion |
| CN114573755A (en) * | 2022-05-05 | 2022-06-03 | 山东奥赛新材料有限公司 | Preparation method of cationic emulsifier for rosin size |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115746201A (en) | 2023-03-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4110521A (en) | Continuous polymerization apparatus and process | |
| US7265190B2 (en) | Process and apparatus for production of water-absorbent resin | |
| CN1121417C (en) | Prepn. of emulsion homopolymers and copolymers and device therefor | |
| US4196272A (en) | Continuous process for the preparation of an acrylic acid-methyl acrylate copolymer in a tubular reactor | |
| CN103113504B (en) | Organic fluorine modified solid water-borne acrylic resin and preparation method thereof | |
| CN101921349A (en) | Radiation polymerization method of continuous hydrous dispersoids of unsaturated monomer | |
| CN102443090A (en) | Synthetic method for fluororubber | |
| CN111234081A (en) | Low-molecular-weight narrow-distribution styrene-maleic anhydride copolymer and preparation method thereof | |
| CN108690155A (en) | The method that polyacrylamide is prepared by acrylamide using microreactor | |
| Bayer et al. | Micro mixing effects in continuous radical polymerization | |
| CN115746201B (en) | Synthetic method of chlorine-free cationic rosin size emulsifier | |
| CN110964147A (en) | Gel-free amphoteric dry strength agent and preparation method thereof | |
| CN1031582C (en) | Prepn. of copolymer containing dimethyl-dipropylidene ammonium chloride and acrylamide | |
| CN103304714A (en) | Preparation method of instant ultra-high molecular weight polyacrylamide dry powder | |
| EP2617742B1 (en) | N-vinyl lactam polymer and method for producing same | |
| CN213977502U (en) | Continuous production device of hydroxyl acrylic resin | |
| US4331792A (en) | Continuous process for production of copolymer of an alkali metal vinyl sulfonate and acrylic acid | |
| CN113429557B (en) | Continuous preparation method of low-viscosity polyether polyol | |
| CN109206549B (en) | Cationic free radical polymerization emulsion for metal surface treatment field and preparation method thereof | |
| CN106317306B (en) | A kind of preparation method of cationic polyacrylamide | |
| CN101519471A (en) | Emulsion-polymerizing preparation method of chlorinated polyether resin | |
| US4559202A (en) | Apparatus for preparing polymer solutions | |
| CN112552439B (en) | Cationic polymer and preparation method thereof | |
| CN101381458B (en) | Method for preparing dimethyldiallyl ammonium chloride and sulfur dioxide co-polymer PAS | |
| CN107955107B (en) | Method for preparing star polyacrylamide by single electron transfer living radical polymerization |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |