CN101323652B - Preparing methods of polyisoprene emulsion and rubber thereof - Google Patents
Preparing methods of polyisoprene emulsion and rubber thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a polyisoprene rubber latex and a polyisoprene rubber, wherein, the polyisoprene rubber latex is obtained by the emulsion polymerization of isoprene and then aggregated by breaking emulsion to obtain the polyisoprene rubber. The technological process for preparing latex in the invention is easy to control and the obtained polyisoprene rubber latex has stable quality; the crude rubber has good physical and mechanical properties and can meet the requirements of multiple purposes and the diversified demands of the market. The polyisoprene rubber prepared by the invention is mixed and vulcanized with a processing method commonly-adopted by the production of rubber and can be used for manufacturing rubber products, such as various tires, triangular belts, conveyer belts, sealing rings, rubber tubes, rubber shoes and buffering blocks.
Description
Technical field
The present invention relates to the preparation method of methods of polyisoprene emulsion and rubber thereof.Specifically be that isoprene is obtained methods of polyisoprene emulsion by letex polymerization, assemble obtaining rubber again through breakdown of emulsion, belong to polymer chemistry, Polymer Physics, colloid chemistry, rubber physics and chemical field.
Background technology
Isoprene is a kind of important unsaturated and conjugated diolefin, and the preparation isoprene has that olefine aldehydr is synthetic, produces C in iso-pentane and dehydrogenation of isoamylene, the ethene refining in the industry
5Production methods such as cut separation, acetylenic ketone method, wherein C
5The development of cut partition method is very fast.Industrial isoprene monomer mainly is to prepare polyisoprene by solution catalyzing or ionic polymerization, is used for substituting natural rubber.Polyisoprene also can become emulsion by emulsion polymerization prepared, uses as latex product.The preparation method of current methods of polyisoprene emulsion is outer emulsion process, it promptly is medium with the organic solvent, adopt methods such as anionoid polymerization, polycoordination synthetic along 1,4-polyisoprene solution, again with polyisoprene solution and water, an amount of emulsifying agent through high-speed stirring emulsification, remove and concentrate behind the solvent and get.
CN 1324874A discloses the method that a kind of acquisition has the polyisoprene rubber of high-cis 1,4 linkage content, and it is by polymerization and getting in the organic hydrocarbon solvent of inertia such as the organophosphate of monomer isoprene, rare earth metal, aluminum alkyls.CN 85102250B discloses a kind of isoprene prepares polyisoprene rubber by mass polymerization under the rare earth catalyst effect method.U.S. Pat 3285869 discloses a kind of preparation method of methods of polyisoprene emulsion, promptly obtains polyisoprene solution with Ziegler-Nata catalyzer or lithium catalyst by solution polymerization, disperses the back desolventizing with emulsifier solution emulsification then.U.S. Pat 3971746 discloses a kind of methods of polyisoprene emulsion of carboxylation, and it is to introduce 0.03%～20% carboxyl when solution polymerization, has improved the stability after the emulsification.
The above-mentioned patent of isoprene aspect synthetic rubber that relate to, its disclosed preparation method all is ionic polymerization or the polycoordinations in organic solution, belong to solution polymerization and polyisoprene rubber (abbreviation contains intermingle with isoamyl glue), it is good that this contains intermingle with the product properties that isoamyl glue makes.But polymerization process needs to do medium with a large amount of organic solvents, not only has problem of environmental pollution, security hidden trouble, and also organic solvent removes, to reclaim technology loaded down with trivial details.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of polyisoprene rubber emulsion.This preparation method prepares the control of emulsion technological process easily, the polyisoprene rubber product emulsion steady quality that obtains.
Another object of the present invention provides a kind of preparation method of polymerization synthetic polyisoprene.This preparation method is that the polyisoprene rubber emulsion is good through the rubber physical and mechanical properties that cohesion, washing, drying obtain, and can satisfy multi-purpose needs, satisfies the demand of market diversification.
Preparation method as the polyisoprene rubber emulsion of first aspect present invention, be to be monomer with the isoprene, with anionic emulsifier, dispersion agent is emulsification system, adopts redox initiation system, obtains stable polyisoprene rubber emulsion through free-radical emulsion polymerization under normal pressure.
Because the purity of isoprene is bigger to the rate of polymerization influence, therefore, in the preparation method of polyisoprene rubber emulsion of the present invention, the purity of isoprene monomer will reach more than 98%.
The present invention selects the anionic emulsifier with better emulsifying capacity for use, and described anionic emulsifier includes but not limited to: alkyl-sulphate, alkylsulfonate, alkylbenzene sulfonate, a kind of in the hard soap.Described alkyl-sulphate is preferably sodium lauryl sulphate.Described alkylsulfonate is preferably a kind of in sodium laurylsulfonate and the succsinic acid alkyl ester sodium sulfonate.Described alkylbenzene sulfonate is preferably Sodium dodecylbenzene sulfonate.Described hard soap is preferably sodium oleate, potassium oleate, a kind of in the nilox resin acid potash soap.
The consumption of described anionic emulsifier is 2～12wt% of isoprene monomer total amount, and preferred consumption is 4～10wt%.
The adding of dispersion agent of the present invention can make polymerization process more steady, the transformation efficiency height, and emulsion-stabilizing, gel is few, and polymerization efficiency improves.Described dispersion agent is selected condensation formaldehyde naphthalene sulfonic acid salt for use, and this condensation formaldehyde naphthalene sulfonic acid salt has Dispersant MF, dispersion agent NF and the dispersion agent N of commercial grade.
Described dispersant dosage is 0.05～1wt% of isoprene monomer total amount, and preferred consumption is 0.1～0.8wt%.
Oxygenant consumption in the redox initiation system that the present invention adopts is with selecting for use kind different, but consumption should be controlled between the 0.2-2wt% of isoprene monomer total amount, and preferable amount is 0.2-1wt%.The reductive agent consumption is with selecting for use kind different, but general consumption is the 0.2-2wt% of isoprene monomer total amount, and preferred consumption is 0.2-1wt%.
Described oxygenant is selected superoxide for use, and described superoxide adopts a kind of or both mixing in acyl peroxide class, the hydroperoxide kind.Described acyl peroxide class is one or more the mixing in dibenzoyl peroxide, lauroyl peroxide, the decanoyl peroxide.Be preferably dibenzoyl peroxide.
Described hydroperoxide kind is a kind of in hydrogen peroxide, pinane hydrogen peroxide, tertbutyl peroxide, hydrogen phosphide cumene, di-isopropylbenzene hydroperoxide, hydrogen peroxide tri-isopropyl benzene, t-butyl hydroperoxide isopropyl benzene, the hydrogen peroxide chloro diisopropylbenzene(DIPB) or both and both above mixing.Be preferably tertbutyl peroxide, di-isopropylbenzene hydroperoxide.
Described reductive agent is one or both and the two or more mixing in sodium bisulfite, sodium formaldehyde sulfoxylate, Sulfothiorine, V-Brite B, ferrous sulfate, iron protochloride, the xitix.
In the preparation method of polyisoprene rubber emulsion of the present invention, can also select the molecular weight of molecular weight regulator control polyisoprene for use.The consumption of described molecular weight regulator is monomer total amount 0.05-0.8wt%, and preferred consumption is 0.1-0.5wt%.
Above-mentioned molecular weight regulator be just-DDM dodecyl mercaptan, just-14 carbon mercaptan, just-16 a kind of or two kinds and the two or more mixing in carbon mercaptan, uncle-DDM dodecyl mercaptan, uncle-14 carbon mercaptan, the uncle-16 carbon mercaptan.Preferably just-DDM dodecyl mercaptan, uncle-DDM dodecyl mercaptan.
Tank reactor is adopted in methods of polyisoprene emulsion polymerization of the present invention, carries out under normal pressure; According to the temperature of reaction difference, be divided into two kinds of hot polymerization reaction and cold poly-reactions: wherein the hot polymerization temperature of reaction is 25～32 ℃, and total reaction time is between 25～40 hours; Cold poly-temperature of reaction is 5～15 ℃, and total reaction time is between 30～60 hours.When reaction conversion ratio reaches 85% when above, add terminator, anti-aging agent makes reaction terminating; Behind the reaction terminating, polyisoprene latex is sent into degassing still, remove unreacted monomer through flash distillation, gas.
The terminator that above-mentioned polyreaction adopted is common compound with terminating free-radical polymerisation processes ability, a kind of in quinhydrones, Resorcinol, p-ten.-butylcatechol, MEHQ, diethanolamine, the Sodium dimethyldithiocarbamate 40min.Be preferably diethanolamine, Sodium dimethyldithiocarbamate 40min.The consumption of terminator is the 0.05-0.5wt% of monomer total amount, and preferred consumption is 0.1-0.3wt%.
The anti-aging agent that above-mentioned polyreaction adopted is a kind of in phenols, amine, sulfurous esters, the thioesters class anti-aging agent, and these all are applicable to emulsion of the present invention.Be preferably phenolic type antioxidant, described phenolic type antioxidant is antioxidant 264, antioxidant 2246, anti-aging agent 246, a kind of in antioxidant SP, the antioxidant d.The consumption of anti-aging agent is the 0.2-4wt% of monomer total amount, and preferred consumption is 0.3-2wt%.
As the polymerization synthetic polyisoprene of second aspect present invention be by the methods of polyisoprene emulsion after the degassing through cohesion, filter, washing, dry and get, specifically comprise following steps:
(1) add flocculation agent in methods of polyisoprene emulsion, stable methods of polyisoprene emulsion is the unstability cohesion under the flocculation agent effect, generates the slurries that contain the rubber blob of viscose;
(2) filter, blob of viscose is separated from slurries;
(3) washing: blob of viscose is changed in the washing bath, wash with water;
(4) filter: blob of viscose is separated from the slurries of washing;
(5) blob of viscose dewater, drying.
Flocculation agent of the present invention is selected a kind of in mineral acid, metal-salt, the polymeric flocculant for use.
Described mineral acid is selected a kind of in hydrochloric acid, sulfuric acid, the nitric acid for use, is preferably sulfuric acid.
Described metal-salt is a kind of in 1 valency, divalent, the 3 valency metal-salts.Described 1 valency metal-salt is Na
+Salt, divalent metal-salt are Mg
2+, Ca
2+, Zn
2+Salt, 3 valency metal-salts are Al
3+Salt.Described Na
+Salt is NaCl; Described Mg
2+Salt is MgCl
2, MgSO
4Described Ca
2+Salt is CaCl
2, Ca (NO
3)
2Described Zn
2+Salt is Zn (NO
3)
2Described Al
3+Salt is AlCl
3, Al
2(SO
4)
3The preferred MgSO of described metal-salt
4, CaCl
2, Al
2(SO
4)
3
Described polymeric flocculant is a polyacrylamide.
In preferred embodiment of the present invention, flocculation agent selects excellent CaCl
2With vitriolic combination, wherein CaCl
2As main flocculation agent, its consumption is 8～40wt% of emulsion total amount, generally is made into weight concentration and is 5～30% the aqueous solution and use, and preferably is made into weight concentration and is 10～20% the aqueous solution and use; Sulfuric acid is used for regulating the pH of slurries as coagulant aids, and pH is controlled at 5～8, preferably is controlled at 5.5～7.
In above-mentioned steps (2), slurries and newborn polyisoprene rubber blob of viscose are sent into the rinse bath or the service sink that have whipping appts then by vibratory screening apparatus or vibrating bed filtering separation.
In above-mentioned steps (3), blob of viscose is admitted to the rinse bath or the service sink that have whipping appts and washs, to remove soluble impurities such as a large amount of flocculation agent, emulsifying agent.
In above-mentioned steps (4), the slurries of washing and blob of viscose are by vibratory screening apparatus or vibrating bed filtering separation.
Contain a large amount of moisture content owing to filter the blob of viscose that obtains, further dehydrate.Therefore in above-mentioned steps (5), moisture blob of viscose is sent into whizzer and is dewatered, and the blob of viscose after the dehydration is sent into the moisture eliminator drying, promptly gets rubber after the drying.Described whizzer is preferably horizontal centrifuge, and the preferred dynamically moisture eliminator of described moisture eliminator includes but not limited to fluidizing drying bed, spiral flash distillation dryer.
Generally, in above-mentioned steps (2) and step (4), send knockouts back to through the slurries after vibratory screening apparatus or the vibrating bed filtration, flocculation agent wherein can recycle.The washing water that can not utilize are delivered to treatment tank, treated qualified back discharging.
The polyisoprene rubber that the present invention makes adopts the general working method of rubber to carry out mixing and sulfuration.By 100 parts of newborn polyisoprene rubbers, 1.5 parts of stearic acid, 1 part of altax; 5 parts in zinc oxide; The proportioning that 40 parts of semi-reinforcing hydrocarbon blacks and sulphur are 1.5 parts carry out in two roller mills mixing after, 145 ℃ of insulations are 50 minutes under certain pressure on the dull and stereotyped rubber vulcanizing machine, the gained rubber sample carries out performance test by national standard.The polyisoprene rubber that the present invention makes can be used for various tires, wire belt, travelling belt, sealing-ring, sebific duct, rubber overshoes and buffer block rubber item.
Embodiment
Following examples are detailed description of the invention, can not be interpreted as it is qualification to technical solution of the present invention.
Example 1
To logical nitrogen at the bottom of the polymeric kettle after 30 minutes, press in the table 1 each set of dispense than in reactor, adding 100 parts of deionized waters, whole SBLS, EDTA, MF and NaHCO
3, stirring and dissolving is made into water.IP, CHP all add the monomer still, and stirring and dissolving is made into oil phase.45 parts of deionized waters, whole FeSO
4Add the reductive agent still, stirring and dissolving is made into the aqueous solution.Control still temperature begins to drip IP at 28 ℃～32 ℃, drips off at 8 ~ 10 hours.The FeSO of synchronous dropping 80%
4The aqueous solution dripped off at 8～10 hours hours.Reach at 60% o'clock at transformation efficiency, add the FeSO of residue 20%
4The aqueous solution.Continue reaction 10～15 hours,, add 0.2 part of diethanolamine, 1 part of antioxidant 264 when transformation efficiency reaches 85% when above.Behind the reaction terminating, polyisoprene latex is sent into degassing still, remove unreacted monomer, obtain stable white emulsion through flash distillation, gas.Degassing condition: 50～70 ℃ of temperature, vacuum tightness-0.08～-0.1MPa, 2～3 hours time.The solid content that obtains emulsion is 35.7%, and pH 6.6, particle diameter 172nm.
Drop into 80 parts of emulsions in knockouts, 20 parts of deionized waters stir.Drop into CaCl to the flocculation agent still
220 parts, 150 parts of deionized waters, stirring and dissolving.To knockouts, add CaCl from the flocculation agent still
2Solution adds in 40～60min.Adition process keeps knockouts to be in whipped state, and regulates the interior slurries pH of knockouts 5～7 with 0.5% sulphuric acid soln.Cohesion finished, and slurries are sent into rinse bath, with 2～3 times clear water agitator treatings 1～1.5 hour.Mixture after the washing filters through vibratory screening apparatus, obtains wet blob of viscose.Wet blob of viscose is sent into horizontal centrifuge dehydration 20～30min through conveying belt, send into spiral flash distillation dryer drying by feeding screw then, 110～130 ℃ of dryer inlet temperatures, material is the residence time 10～15s in moisture eliminator, can get the dried blob of viscose of water content＜1%.
The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Example 2
Dodecyl Mercaptan in the example 1 is adjusted into 0.15 part, and SBLS is 3.5 parts, and MF is 0.5 part, material consumption such as table 1, and other processing condition are constant.The solid content that obtains emulsion is 36.2%, and pH 7.1, particle diameter 183nm.The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Example 3
Press table 1 and in reactor, add 100 parts of deionized waters after 30 minutes to logical nitrogen at the bottom of the polymeric kettle, all DRS, EDTA, MF and NaHCO
3, stirring and dissolving is made into water.IP, CHP all add the monomer still, and stirring and dissolving is made into oil phase.50 parts of deionized waters, whole FeSO
4Add the reductive agent still, stirring and dissolving is made into the aqueous solution.Control still temperature begins to drip IP at 10 ℃～13 ℃, drips off at 10-15 hour hour.The FeSO of synchronous dropping 80%
4The aqueous solution dripped off at 10 ~ 15 hours hours.Reach at 60% o'clock at transformation efficiency, add the FeSO of residue 20%
4The aqueous solution.Continue reaction 15 ~ 25 hours,, add 0.2 part of diethanolamine, 1 part of antioxidant 264 when transformation efficiency reaches 85% when above.Behind the reaction terminating, polyisoprene latex is sent into degassing still, remove unreacted monomer, obtain stable white emulsion through flash distillation, gas.Degassing condition: 50～70 ℃ of temperature, vacuum tightness-0.08--0.1MPa, 2～3 hours time.The solid content that obtains emulsion is 35.1%, and pH 6.3, particle diameter 185nm.
Drop into 78 parts of emulsions in knockouts, 22 parts of deionized waters stir.Drop into CaCl to the flocculation agent still
216 parts, 140 parts of deionized waters, stirring and dissolving.To knockouts, add CaCl from the flocculation agent still
2Solution adds in 50～60min.Adition process keeps knockouts to be in whipped state, and regulates the interior slurries pH of knockouts 5～7 with 0.5% sulphuric acid soln.Cohesion finished, and slurries are sent into rinse bath, with 2～3 times clear water agitator treatings 1～1.5 hour.Mixture after the washing filters through vibratory screening apparatus, obtains wet blob of viscose.Wet blob of viscose is sent into horizontal centrifuge dehydration 20～30min through conveying belt, send into spiral flash distillation dryer drying by feeding screw then, 110～130 ℃ of dryer inlet temperatures, material is the residence time 10～15s in moisture eliminator, can get the dried blob of viscose of water content＜1%.
The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Example 4
DRS in the example 3 is adjusted into 3 parts, increases by 1 part of SBLS, material consumption such as table 1, other processing condition are constant.The solid content that obtains emulsion is 36.7%, and pH 6.8, particle diameter 173.5nm.The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Example 5
With CaCl in the flocculation agent still in the example 1
2Be adjusted into 17 parts, deionized water is 170 parts.CaCl
2The joining day of solution is extended for 70 minutes, and other processing condition are constant.The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Example 6
With CaCl in the flocculation agent still in the example 3
2Be adjusted into 17 parts, deionized water is 170 parts.CaCl
2The joining day of solution is extended for 70 minutes, and other processing condition are constant.The physical and mechanical properties of gained blob of viscose is as shown in table 2.
Each component and consumption in the polymerization of table 1 methods of polyisoprene emulsion
Table 2 emulsion polyisoprene rubber physical and mechanical properties
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Mooney viscosity, (ML 1+4 100) | 156 | 148 | 72 | 66 | 158 | 67 |
| Breaking tenacity, Mpa | 17.6 | 18.3 | 28.4 | 26.8 | 16.7 | 29.1 |
| Elongation at break, % | 358 | 366 | 574 | 601 | 377 | 547 |
| Shore hardness, A | 79 | 82 | 58 | 51 | 74 | 46 |
Claims (20)
1. the preparation method of polyisoprene rubber emulsion is a monomer with the isoprene, is emulsification system with the anionic emulsifier, adopts redox initiation system, obtains stable polyisoprene rubber emulsion through free-radical emulsion polymerization under normal pressure, it is characterized in that,
Tank reactor is adopted in described methods of polyisoprene emulsion polymerization, carries out under normal pressure; According to the temperature of reaction difference, be divided into two kinds of hot polymerization reaction and cold poly-reactions;
The hot polymerization temperature of reaction is 25～32 ℃, and total reaction time is between 25～40 hours; After 30 minutes, in reactor, add 100 parts of deionized waters, all 4 parts of Sodium dodecylbenzene sulfonate SBLS, diethylamine tetraacethyl EDTA0.2 part, 0.3 part of Dispersant MF and NaHCO to logical nitrogen at the bottom of the polymeric kettle by each set of dispense ratio
31.3 part, stirring and dissolving is made into water; Isoprene IP100 part, hydrogen phosphide cumene CHP0.4 part, all add the monomer still, stirring and dissolving is made into oil phase; 45 parts of deionized waters, whole FeSO
40.4 part adding reductive agent still, it is standby that stirring and dissolving is made into the aqueous solution; Control still temperature begins to drip IP at 28 ℃～32 ℃, drips off at 8～10 hours, drips the FeSO of 80% preparation synchronously
4The aqueous solution dripped off at 8～10 hours, reached at 60% o'clock at transformation efficiency, added the FeSO of the preparation of residue 20%
4The aqueous solution continues reaction 10-15 hour;
Or cold poly-temperature of reaction is 5～15 ℃, and total reaction time is between 30～60 hours; To leading to nitrogen at the bottom of the polymeric kettle after 30 minutes, in reactor, press each set of dispense than adding 100 parts of deionized waters, 3 parts of nilox resin acid potash soap DRS and 1 part of Sodium dodecylbenzene sulfonate SBLS or 4 parts of whole nilox resin acid potash soap DRS, 0.2 part of diethylamine tetraacethyl EDTA, 0.3 part of Dispersant MF and NaHCO
31.3 part, stirring and dissolving is made into water; Isoprene IP100 part, hydrogen phosphide cumene CHP0.4 part, all add the monomer still, stirring and dissolving is made into oil phase; 50 parts of deionized waters, whole FeSO
40.4 part adding reductive agent still, it is standby that stirring and dissolving is made into the aqueous solution; Control still temperature begins to drip IP at 10 ℃～13 ℃, drips off at 10～15 hours, drips the FeSO of 80% preparation synchronously
4The aqueous solution dripped off at 10～15 hours, reached at 60% o'clock at transformation efficiency, added the FeSO of the preparation of residue 20%
4The aqueous solution continues reaction 15-25 hour;
And, when polymerization conversion reaches 85%, add 0.2 part of diethanolamine, 1 part of antioxidant 264 makes reaction terminating; Behind the reaction terminating, polyisoprene latex is sent into degassing still, remove unreacted monomer through flash distillation, gas.
2. preparation method as claimed in claim 1 is characterized in that the purity of described isoprene monomer reaches more than 98%.
3. preparation method as claimed in claim 1 is characterized in that, adopts the molecular weight of molecular weight regulator control polyisoprene, and consumption is the 0.05-0.8wt% of isoprene monomer total amount.
4. preparation method as claimed in claim 3, it is characterized in that, described molecular weight regulator be just-DDM dodecyl mercaptan, just-14 carbon mercaptan, just-16 one or more kinds of mixing in carbon mercaptan, uncle-DDM dodecyl mercaptan, uncle-14 carbon mercaptan, the uncle-16 carbon mercaptan.
5. the polyisoprene rubber emulsion of the preparation method's preparation that utilizes the described polyisoprene rubber emulsion of claim 1 prepares the method for polymerization synthetic polyisoprene, it is characterized in that, be by the methods of polyisoprene emulsion after the degassing through cohesion, filter, washing, dry and get, specifically comprise following steps:
(1) preparation method according to the described polyisoprene rubber emulsion of claim 1 prepares methods of polyisoprene emulsion;
(2) add flocculation agent in methods of polyisoprene emulsion, stable methods of polyisoprene emulsion is the unstability cohesion under the flocculation agent effect, generates the slurries that contain the rubber blob of viscose;
(3) filter, blob of viscose is separated from slurries;
(4) washing: blob of viscose is changed in the washing bath, wash with water;
(5) filter: blob of viscose is separated from the slurries of washing;
(6) blob of viscose dewater, drying.
6. preparation method as claimed in claim 5 is characterized in that, described flocculation agent is a kind of in mineral acid, metal-salt, the polymeric flocculant.
7. preparation method as claimed in claim 6 is characterized in that, described mineral acid is a kind of in hydrochloric acid, sulfuric acid, the nitric acid.
8. preparation method as claimed in claim 6 is characterized in that, described metal-salt is a kind of in 1 valency, divalent, the 3 valency metal-salts.
9. preparation method as claimed in claim 8 is characterized in that, described 1 valency metal-salt is NaCl.
10. preparation method as claimed in claim 8 is characterized in that, described divalent metal-salt is MgCl
2, MgSO
4, CaCl
2, Ca (NO
3)
2And Zn (NO
3)
2
11. preparation method as claimed in claim 8 is characterized in that, described 3 valency metal-salts are AlCl
3, Al
2(SO
4)
3
12. preparation method as claimed in claim 6 is characterized in that, described metal-salt is MgSO
4, CaCl
2, Al
2(SO
4)
3In a kind of.
13. preparation method as claimed in claim 6 is characterized in that, described polymeric flocculant is a polyacrylamide.
14. preparation method as claimed in claim 5 is characterized in that, described flocculation agent is CaCl
2With vitriolic combination, wherein CaCl
2As main flocculation agent, its consumption is 8～40wt% of emulsion total amount, is made into weight concentration and is 5～30% the aqueous solution and use, and described sulfuric acid is used for regulating the pH of slurries as coagulant aids, and pH is controlled at 5～8.
15. preparation method as claimed in claim 5 is characterized in that, in above-mentioned steps (3), slurries and polyisoprene rubber blob of viscose are sent into the rinse bath or the service sink that have whipping appts then by vibratory screening apparatus or vibrating bed filtering separation.
16. preparation method as claimed in claim 5 is characterized in that, in above-mentioned steps (4), blob of viscose is admitted to the rinse bath or the service sink that have whipping appts and washs, to remove a large amount of flocculation agent, emulsifying agent soluble impurity.
17. preparation method as claimed in claim 5 is characterized in that, in above-mentioned steps (5), washing slurries and blob of viscose are by vibratory screening apparatus or vibrating bed filtering separation.
18. preparation method as claimed in claim 5 is characterized in that, in above-mentioned steps (6), moisture blob of viscose is sent into horizontal centrifuge and is dewatered, and the blob of viscose after the dehydration is sent into dynamic moisture eliminator drying, promptly gets rubber after the drying.
19. preparation method as claimed in claim 18 is characterized in that, that described dynamic moisture eliminator comprises is fluidizing drying bed, a kind of in the spiral flash distillation dryer.
20. as claim 15 or 17 described preparation methods, it is characterized in that, in above-mentioned steps (3) and step (5), send knockouts back to through the slurries after vibratory screening apparatus or the vibrating bed filtration, flocculation agent wherein can recycle, the washing water that can not utilize are delivered to treatment tank, treated qualified back discharging.
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| CN112898621B (en) * | 2021-03-16 | 2023-04-25 | 青岛瑞诺化工有限公司 | Emulsifier, preparation method thereof and application of emulsifier in latex foaming product |
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