CN103113598A - Preparation method of anionic rosin trimethylolpropane ester emulsion - Google Patents
Preparation method of anionic rosin trimethylolpropane ester emulsion Download PDFInfo
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- CN103113598A CN103113598A CN2013100768596A CN201310076859A CN103113598A CN 103113598 A CN103113598 A CN 103113598A CN 2013100768596 A CN2013100768596 A CN 2013100768596A CN 201310076859 A CN201310076859 A CN 201310076859A CN 103113598 A CN103113598 A CN 103113598A
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- Prior art keywords
- rosin
- anionic
- temperature
- aqueous solution
- trimethylolpropane
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- 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 66
- 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 66
- 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 66
- -1 trimethylolpropane ester Chemical class 0.000 title claims abstract description 33
- 239000000839 emulsion Substances 0.000 title claims abstract description 22
- 125000000129 anionic group Chemical group 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 229920006318 anionic polymer Polymers 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000005886 esterification reaction Methods 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 13
- 239000000498 cooling water Substances 0.000 claims description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- 239000008234 soft water Substances 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- 229920001577 copolymer Polymers 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 230000001143 conditioned effect Effects 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- JXAZAUKOWVKTLO-UHFFFAOYSA-L sodium pyrosulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OS([O-])(=O)=O JXAZAUKOWVKTLO-UHFFFAOYSA-L 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 2
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical group CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 claims description 2
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 claims description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 2
- 239000001639 calcium acetate Substances 0.000 claims description 2
- 235000011092 calcium acetate Nutrition 0.000 claims description 2
- 229960005147 calcium acetate Drugs 0.000 claims description 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 2
- 235000010331 calcium propionate Nutrition 0.000 claims description 2
- 239000004330 calcium propionate Substances 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920000151 polyglycol Polymers 0.000 claims description 2
- 239000010695 polyglycol Substances 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 2
- 230000000996 additive effect Effects 0.000 abstract 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 abstract 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000008267 milk Substances 0.000 description 4
- 210000004080 milk Anatomy 0.000 description 4
- 235000013336 milk Nutrition 0.000 description 4
- 239000008233 hard water Substances 0.000 description 3
- 239000000693 micelle Substances 0.000 description 3
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Abstract
The invention discloses a preparation method of an anionic rosin trimethylolpropane ester emulsion, and relates to the technical field of chemical industry. The preparation method comprises the following steps of: firstly, adding rosin, trimethylolpropane and a catalyst E to a reactor, mixing under the protection of nitrogen, then increasing the temperature, and carrying out esterification reaction twice to obtain rosin trimethylolpropane ester, mixing and reacting a sodium hydroxide aqueous solution of which the content is 50% and an additive R aqueous solution of which the content is 30 to 50%, adjusting the pH value of a mixture of the sodium hydroxide aqueous solution and the additive R aqueous solution by using sodium hydrogen sulfate to obtain an anionic polymer rosin emulsifier, and carrying out reaction on the anionic polymer rosin emulsifier and rosin trimethylolpropane ester, thus obtaining the anionic rosin trimethylolpropane ester emulsion. In comparison with the prior art, the anionic rosin trimethylolpropane ester emulsion is small in colloidal particles, difficult in agglomeration, less in foamability, stable in coating, and capable of keeping a good viscous force while effectively improving the initial viscous force and the stripping strength of an adhesive, and meets customer requirements.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of preparation method of anionic rosin trihydroxymethylpropanyl ester emulsion.
Background technology
Leading status is being captured in rosin production and the rosin deep processing of China in the world always, flourish along with the Gum Rosin industry, the various product of Gum Rosin has been widely used in the industries such as tackiness agent, coating, papermaking, printing ink, rubber, batik, food.But because the tempo of recent domestic petroleum resin is very fast, be subjected to seasonal effect less due to the starting material of petroleum resin sources again, acquisition cost is relatively low, causes petroleum resin to have larger advantage on price, thereby has impacted original market of Gum Rosin.In recent years again at a time when world economy depressed makes rosin deep processing industry be subject to a certain extent strike.But we have also seen the advantage place of Gum Rosin, and from overall performance, Gum Rosin is used more extensive than petroleum resin, and effect is more superior.The raw material sources of Gum Rosin are in renewable resources rosin, but China's pine tree resin tapping amount only reaches 50% of existing pine tree resin tapping amount at present, the relatively day by day exhausted more aobvious advantage of petroleum resources.From the long term growth prospect, rosin and deep processing industry thereof meet the ambitious goal of Sustainable development, more have good development prospect.
Market of Adhesives both domestic and external relates to the packing of pencil, books customized, and furniture bonding, all tackiness agent are all lived closely bound uply with us basically, are directly connected to our health.And inflammable, explosive, volatile, the toxic solvents such as the containing benezene that existing tackiness agent has, ester class, ketone, and the rosin milk of tackiness agent can not take into account each performance index, and foaming is large, little to hard water and temperature tolerance, easily cohesion, micelle is large, is coated with unstable.
Summary of the invention
The invention provides a kind of preparation method of anionic rosin trihydroxymethylpropanyl ester emulsion, it can solve existing rosin milk can not take into account each performance index, and foaming is large, little to hard water and temperature tolerance, easily cohesion, micelle is large, is coated with unsettled problem.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
The preparation method of anionic rosin trihydroxymethylpropanyl ester emulsion of the present invention, its preparation process is as follows:
A, add rosin, TriMethylolPropane(TMP) and catalyzer E in reactor, the weight ratio of TriMethylolPropane(TMP) and rosin is 1.2-1.6:10, the weight ratio of catalyzer E and rosin is 0.1-0.25:100, mixed in 180 ℃ under the protection of nitrogen, then be warmed up to 210 ℃, and be incubated 2 hours and carry out the partial esterification reaction, be warmed up to again 250 ℃-255 ℃ after 2 hours finish, and be incubated 5-8 hour and carry out esterification, namely obtain the rosin trihydroxymethylpropanyl ester, check in insulation softening temperature and the acid number whether color of resin is deepened and detected resin after 5 hours;
B, formulation content are the auxiliary agent R aqueous solution that 50% aqueous sodium hydroxide solution and content are 30-50%, under agitation condition, mode take the weight ratio of aqueous sodium hydroxide solution and the auxiliary agent R aqueous solution as 1:5 adds the auxiliary agent R aqueous solution to aqueous sodium hydroxide solution, mixed complete rear stirring 60 minutes, drip sodium pyrosulfate after reaction finishes, regulate the pH value of mixed solution, make pH value be controlled at 7-10, use simultaneously cooling water circulation control temperature of reaction, adjusting temperature is 70 ℃-75 ℃; Adjustment is completed, and filters, and obtains anionic polymer rosin emulsifying agent;
C, the temperature of conditioned reaction still is under the condition of 100 ℃-105 ℃, the anionic polymer rosin emulsifying agent of B step gained and the ratio of rosin trihydroxymethylpropanyl ester take weight ratio as 1.5-2:10 of A step gained are progressively added anionic polymer rosin emulsifying agent to the rosin trihydroxymethylpropanyl ester, mix 20 minutes, cool to 97 ℃-100 ℃, add again 90 ℃ of hot soft water to make the resin phase inversion, progressively add 90 ℃ of hot soft water to calculate after phase inversion and adjust emulsion solid content, adjust complete, use cooling water temperature, temperature of cooling water and the still temperature temperature difference are no more than 30 ℃, namely get anionic rosin trihydroxymethylpropanyl ester emulsion.
In technique scheme, scheme is more specifically: described catalyzer E is esterifying catalyst, and described esterifying catalyst is one or more the mixture in phosphoric acid, Hypophosporous Acid, 50, calcium propionate, calcium hydroxide, calcium acetate, Quilonum Retard, zinc oxide and magnesium oxide; Described auxiliary agent R is polymeric surface active agent, and described polymeric surface active agent is one or more the mixture in Styrene And Chloroalkyl Acrylates salt copolymer, methacrylic acid Soxylat A 25-7-acrylate multipolymer, methyl thiazolinyl polyethenoxy ether, isopentene group polyethers, poly glycol monomethyl ether (CH3O (CH2CH2O) nH) and allyl polyethenoxy ether (CH2=CHCH2O (CH2CH2O) nH).
Owing to adopting technique scheme, the present invention has following beneficial effect:
Because the present invention prepares anionic rosin trihydroxymethylpropanyl ester emulsion with the emulsification of anionic polymer rosin emulsifying agent take rosin and TriMethylolPropane(TMP) after raw material carries out esterification, make the product emulsion foaminess little, large to hard water and temperature tolerance, be difficult for cohesion, micelle is little, and coating is stable; Use than the rosin trihydroxymethylpropanyl ester of high softening-point as basic resin, make emulsion keep the good viscous force of holding in the initial bonding strength that increases substantially tackiness agent and peeling force, the rosin milk that has solved original adhesive industry can not be taken into account the shortcoming of each performance index.
Embodiment
The invention will be further described below in conjunction with specific examples:
Embodiment 1-
Its making step is:
A, add 5400 kilograms of rosin, 648 kilograms of TriMethylolPropane(TMP)s and 5.4 kilograms of phosphoric acid and zinc oxide as esterifying catalyst in reactor, mixed in 180 ℃ under the protection of nitrogen, then be warmed up to 210 ℃, and be incubated 2 hours and carry out the partial esterification reaction, be warmed up to again 250 ℃-255 ℃ after 2 hours finish, and be incubated 5-8 hour and carry out esterification, namely obtain the rosin trihydroxymethylpropanyl ester, check in insulation softening temperature and the acid number whether color of resin is deepened and detected resin after 5 hours; In the situation that color is not deepened, softening temperature and acid number are more near the center of span of control, and rosin TriMethylolPropane(TMP) resin is unreasonable thinks;
The aqueous sodium hydroxide solution of B, formulation content 50% and content are the Styrene And Chloroalkyl Acrylates salt copolymer as polymeric surface active agent of 30-50%, under agitation condition, mode take the weight ratio of aqueous sodium hydroxide solution and Styrene And Chloroalkyl Acrylates salt copolymer as 1:5 adds the Styrene And Chloroalkyl Acrylates salt copolymer to aqueous sodium hydroxide solution, mixed complete rear stirring 60 minutes, after finishing, reaction drips sodium pyrosulfate, regulate the pH value of mixed solution, make pH value be controlled at 7-10, use simultaneously cooling water circulation control temperature of reaction, adjusting temperature is 70 ℃-75 ℃; Adjustment is completed, and filters, and obtains anionic polymer rosin emulsifying agent;
C, the temperature of conditioned reaction still is under the condition of 100 ℃-105 ℃, the anionic polymer rosin emulsifying agent of B step gained and the ratio of rosin trihydroxymethylpropanyl ester take weight ratio as 1.5-2:10 of A step gained are progressively added anionic polymer rosin emulsifying agent to the rosin trihydroxymethylpropanyl ester, mix 20 minutes, cool to 97 ℃-100 ℃, add again 90 ℃ of hot soft water to make the resin phase inversion, progressively add 90 ℃ of hot soft water to calculate after phase inversion and adjust emulsion solid content, adjust complete, use cooling water temperature, temperature of cooling water and the still temperature temperature difference are no more than 30 ℃, namely get anionic rosin trihydroxymethylpropanyl ester emulsion.
Embodiment 2
Its making step is:
A, add calcium hydroxide and the magnesium oxide as esterifying catalyst of 5400 kilograms of rosin, 864 kilograms of TriMethylolPropane(TMP)s and 13.5 kilograms in reactor, mixed in 180 ℃ under the protection of nitrogen, then be warmed up to 210 ℃, and be incubated 2 hours and carry out the partial esterification reaction, be warmed up to again 250 ℃-255 ℃ after 2 hours finish, and be incubated 5-8 hour and carry out esterification, namely obtain the rosin trihydroxymethylpropanyl ester, check in insulation softening temperature and the acid number whether color of resin is deepened and detected resin after 5 hours; In the situation that color is not deepened, softening temperature and acid number are more near the center of span of control, and rosin TriMethylolPropane(TMP) resin is unreasonable thinks;
B, the aqueous sodium hydroxide solution of formulation content 50% and content are the methacrylic acid Soxylat A 25-7 as polymeric surface active agent-acrylate multipolymer of 30-50%, under agitation condition, mode take the weight ratio of aqueous sodium hydroxide solution and methacrylic acid Soxylat A 25-7-acrylate multipolymer as 1:5 adds methacrylic acid Soxylat A 25-7-acrylate multipolymer to aqueous sodium hydroxide solution, mixed complete rear stirring 60 minutes, after finishing, reaction drips sodium pyrosulfate, regulate the pH value of mixed solution, make pH value be controlled at 7-10, use simultaneously cooling water circulation control temperature of reaction, adjusting temperature is 70 ℃-75 ℃, adjustment is completed, and filters, and obtains anionic polymer rosin emulsifying agent,
C, the temperature of conditioned reaction still is under the condition of 100 ℃-105 ℃, the anionic polymer rosin emulsifying agent of B step gained and the ratio of rosin trihydroxymethylpropanyl ester take weight ratio as 1.5-2:10 of A step gained are progressively added anionic polymer rosin emulsifying agent to the rosin trihydroxymethylpropanyl ester, mix 20 minutes, cool to 97 ℃-100 ℃, add again 90 ℃ of hot soft water to make the resin phase inversion, progressively add 90 ℃ of hot soft water to calculate after phase inversion and adjust emulsion solid content, adjust complete, use cooling water temperature, temperature of cooling water and the still temperature temperature difference are no more than 30 ℃, namely get anionic rosin trihydroxymethylpropanyl ester emulsion.
Anionic rosin trihydroxymethylpropanyl ester emulsion technology index of the present invention such as table one:
| Index | Scope |
| Outward appearance | White milk sap |
| Viscosity (30 ℃), mPas | 200-800 |
| PH value | 7-10 |
| Solids content | 58%-62% |
| Stability | Demixing phenomenon did not appear in 180 days |
Claims (2)
1. the preparation method of an anionic rosin trihydroxymethylpropanyl ester emulsion, it is characterized in that: its preparation process is as follows:
A, add rosin, TriMethylolPropane(TMP) and catalyzer E in reactor, the weight ratio of TriMethylolPropane(TMP) and rosin is 1.2-1.6:10, the weight ratio of catalyzer E and rosin is 0.1-0.25:100, mixed in 180 ℃ under the protection of nitrogen, then be warmed up to 210 ℃, and be incubated 2 hours and carry out the partial esterification reaction, be warmed up to again 250 ℃-255 ℃ after 2 hours finish, and be incubated 5-8 hour and carry out esterification, namely obtain the rosin trihydroxymethylpropanyl ester, check in insulation softening temperature and the acid number whether color of resin is deepened and detected resin after 5 hours;
B, formulation content are the auxiliary agent R aqueous solution that 50% aqueous sodium hydroxide solution and content are 30-50%, under agitation condition, mode take the weight ratio of aqueous sodium hydroxide solution and the auxiliary agent R aqueous solution as 1:5 adds the auxiliary agent R aqueous solution to aqueous sodium hydroxide solution, mixed complete rear stirring 60 minutes, drip sodium pyrosulfate after reaction finishes, regulate the pH value of mixed solution, make pH value be controlled at 7-10, use simultaneously cooling water circulation control temperature of reaction, adjusting temperature is 70 ℃-75 ℃; Adjustment is completed, and filters, and obtains anionic polymer rosin emulsifying agent;
C, the temperature of conditioned reaction still is under the condition of 100 ℃-105 ℃, the anionic polymer rosin emulsifying agent of B step gained and the ratio of rosin trihydroxymethylpropanyl ester take weight ratio as 1.5-2:10 of A step gained are progressively added anionic polymer rosin emulsifying agent to the rosin trihydroxymethylpropanyl ester, mix 20 minutes, cool to 97 ℃-100 ℃, add again 90 ℃ of hot soft water to make the resin phase inversion, progressively add 90 ℃ of hot soft water to calculate after phase inversion and adjust emulsion solid content, adjust complete, use cooling water temperature, temperature of cooling water and the still temperature temperature difference are no more than 30 ℃, namely get anionic rosin trihydroxymethylpropanyl ester emulsion.
2. the preparation method of anionic rosin trihydroxymethylpropanyl ester emulsion according to claim 1, it is characterized in that: described catalyzer E is esterifying catalyst, and described esterifying catalyst is one or more the mixture in phosphoric acid, Hypophosporous Acid, 50, calcium propionate, calcium hydroxide, calcium acetate, Quilonum Retard, zinc oxide and magnesium oxide; Described auxiliary agent R is polymeric surface active agent, and described polymeric surface active agent is one or more the mixture in Styrene And Chloroalkyl Acrylates salt copolymer, methacrylic acid Soxylat A 25-7-acrylate multipolymer, methyl thiazolinyl polyethenoxy ether, isopentene group polyethers, poly glycol monomethyl ether (CH3O (CH2CH2O) nH) and allyl polyethenoxy ether (CH2=CHCH2O (CH2CH2O) nH).
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| CN201310076859.6A CN103113598B (en) | 2013-03-12 | 2013-03-12 | Preparation method of anionic rosin trimethylolpropane ester emulsion |
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| CN201310076859.6A CN103113598B (en) | 2013-03-12 | 2013-03-12 | Preparation method of anionic rosin trimethylolpropane ester emulsion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928853A (en) * | 2017-04-27 | 2017-07-07 | 德庆明亮树脂有限公司 | A kind of production method of water-white tackifying resins |
| CN110157372A (en) * | 2019-06-19 | 2019-08-23 | 南宝树脂（佛山）有限公司 | A kind of one-component PUD glue and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07109360A (en) * | 1993-10-08 | 1995-04-25 | Arakawa Chem Ind Co Ltd | Production of resin emulsion |
| CN102039099A (en) * | 2010-11-08 | 2011-05-04 | 中国林业科学研究院林产化学工业研究所 | Self-emulsification rosinyl surfactant emulsion and preparation method thereof |
-
2013
- 2013-03-12 CN CN201310076859.6A patent/CN103113598B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07109360A (en) * | 1993-10-08 | 1995-04-25 | Arakawa Chem Ind Co Ltd | Production of resin emulsion |
| CN102039099A (en) * | 2010-11-08 | 2011-05-04 | 中国林业科学研究院林产化学工业研究所 | Self-emulsification rosinyl surfactant emulsion and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928853A (en) * | 2017-04-27 | 2017-07-07 | 德庆明亮树脂有限公司 | A kind of production method of water-white tackifying resins |
| CN110157372A (en) * | 2019-06-19 | 2019-08-23 | 南宝树脂（佛山）有限公司 | A kind of one-component PUD glue and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN103113598B (en) | 2014-08-27 |
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