CN107602877A - A kind of preparation method of synthetic guttapercha breast - Google Patents
A kind of preparation method of synthetic guttapercha breast Download PDFInfo
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- CN107602877A CN107602877A CN201710788969.3A CN201710788969A CN107602877A CN 107602877 A CN107602877 A CN 107602877A CN 201710788969 A CN201710788969 A CN 201710788969A CN 107602877 A CN107602877 A CN 107602877A
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- latex
- guttapercha
- synthetic
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- synthetic guttapercha
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- 239000000899 Gutta-Percha Substances 0.000 title claims abstract description 80
- 240000000342 Palaquium gutta Species 0.000 title claims abstract description 80
- 229920000588 gutta-percha Polymers 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 210000000481 breast Anatomy 0.000 title claims description 16
- 239000004816 latex Substances 0.000 claims abstract description 61
- 229920000126 latex Polymers 0.000 claims abstract description 61
- 239000003292 glue Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 238000004945 emulsification Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims description 42
- 239000000839 emulsion Substances 0.000 claims description 18
- 239000003381 stabilizer Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 11
- 239000008346 aqueous phase Substances 0.000 claims description 10
- 238000010008 shearing Methods 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000004807 desolvation Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- -1 alkyl carbon Chemical compound 0.000 claims description 7
- 239000012875 nonionic emulsifier Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- 239000012874 anionic emulsifier Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 238000005292 vacuum distillation Methods 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 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 description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229940096992 potassium oleate Drugs 0.000 claims description 2
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 241000208688 Eucommia Species 0.000 claims 2
- 230000000630 rising effect Effects 0.000 claims 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims 1
- 150000008052 alkyl sulfonates Chemical class 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 239000003599 detergent Substances 0.000 claims 1
- 230000001804 emulsifying effect Effects 0.000 claims 1
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 5
- 230000003993 interaction Effects 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000005548 dental material Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- 239000002245 particle Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- KVNRLNFWIYMESJ-UHFFFAOYSA-N butyronitrile Chemical compound CCCC#N KVNRLNFWIYMESJ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000703 high-speed centrifugation Methods 0.000 description 3
- 229920001084 poly(chloroprene) Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 206010020751 Hypersensitivity Diseases 0.000 description 2
- 208000030961 allergic reaction Diseases 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000013536 elastomeric material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000136 polysorbate Polymers 0.000 description 2
- 239000012781 shape memory material Substances 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229940113124 polysorbate 60 Drugs 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The invention belongs to latex preparation field, discloses a kind of preparation method method of synthetic guttapercha latex.This method includes the preparation of synthetic guttapercha glue, the emulsification of synthetic guttapercha glue, the concentration of the solvent removal and synthetic guttapercha latex of synthetic guttapercha latex.Synthetic guttapercha is made latex by the preparation method of synthetic guttapercha latex disclosed in this invention can realize the dispersed and interface interaction of synthetic guttapercha and filler in the form of wet method refining glue afterwards, its technological process is succinct, and the latex for making to be prepared can be applied to medical bandage, dental material or sealing article etc. and require higher field to latex product security and combination property.
Description
Technical field
The present invention relates to latex preparation field, more particularly to a kind of preparation method of synthetic guttapercha breast.
Background technology
Latex product, particularly disposable emulsion product be widely used to health care, national defense and military, daily life,
The numerous areas such as electron detection, wherein, using the species of disposable glove, quantity as most.PVC, Heveatex, synthetic latex
For preparing the latex products such as gloves, PVC product intensity is high, price is low, is widely used, but poor air permeability, degraded be present
The problems such as difficult circumstances are seriously polluted, have started to eliminate in some countries such as America and Europes, latex product price prepared by Heveatex
Low, performance is good, is widely used in the latex products such as surgical glove, industry and domestic purpose gloves, insulating glove, sheath, but due to
The presence of casein etc., easily causes allergic reaction in natural emulsion；Synthetic latex includes neoprene, butyronitrile, butadiene-styrene rubber and its is total to
Mixed or copolymer, the latex product of preparation, the presence of no albumen and avoid allergic reaction, oil resistant and chemical resistance are excellent
Good, wherein neoprene and butyronitrile latex product have realized industrialization, but recycling and the butyronitrile latex product of polychloroprene latex product
Penetrating odor, restrict and influence the popularization of product, latex product its combination property prepared by synthetic latex still can not be with day
Right latex product compares favourably.The compound with regular structure of synthetic guttapercha, easily crystallization, so being hard material at normal temperatures, when unvulcanized
Used as thermoplastic, be usually used in protecting ware for sports and artificial limb set；After vulcanization, used as thermoelastic material, be usually used in shape
Shape memory material.It can also be used simultaneously with other rubber and plastic blend as elastomeric material；But admittedly when being blended admittedly
Tend not to realize well mixed effect, so the present invention can use wet method refining glue after synthetic guttapercha is made into latex
Form realize the dispersed and interface interaction of synthetic guttapercha and filler.
The content of the invention
In view of this, the invention provides a kind of preparation method of synthetic guttapercha breast, it is intended to solves synthetic guttapercha
The dispersed and interface of synthetic guttapercha and filler can not be realized using the high poor compatibility between filler of crystallinity be present
The problem of effect.
A kind of preparation method of synthetic guttapercha breast, the preparation method of the synthetic guttapercha latex comprise the following steps：
(1.1) synthetic guttapercha is dissolved in 70-80 DEG C of nonpolar saturated alkane, dissolution time 8-10h, prepared
Certain density glue, primary emulsion, assistant for emulsifying agent and stabilizer are added in deionized water, prepare emulsifier aqueous solution；Again
Added with potassium hydroxide or potassium dihydrogen phosphate regulation emulsifying agent and stabilizer in deionized water, prepare emulsifier aqueous solution；Again
With the pH value of potassium hydroxide or potassium dihydrogen phosphate regulation emulsifier aqueous solution to 10.0-12.0；
(1.2) glue is added in emulsifier aqueous solution by profit mass ratio 0.5-1.0, then be pumped into emulsion tank, then
Synthetic guttapercha glue is emulsified with emulsifier aqueous solution by high speed shear method, O/W types synthetic guttapercha breast is made
Liquid；
(1.3) the synthetic guttapercha glue after emulsification is pumped into evaporating kettle and distilled, desolvation obtains synthesis Du
Secondary glue dilute latex；
(1.4) the synthetic guttapercha dilute latex after desolvation is concentrated using ultracentrifugal method, obtains 40-
The finished product synthetic guttapercha latex of 80% solid content.
In the step (1.1), nonpolar saturated alkane solvent is selected from hexamethylene, n-hexane, pentamethylene or pentane.
In the step (1.2), emulsifying agent is made up of primary emulsion, assistant for emulsifying agent and stabilizer, by primary emulsion, is helped
Emulsifying agent and stabilizer are prepared and obtained, and the mass ratio of primary emulsion and assistant for emulsifying agent is 1.0-3.0, and the dosage of emulsifying agent is aqueous phase
The 3.0-7.0% of mass percent, the dosage of stabilizer are the 0.01-0.05% of aqueous phase mass percent；In 40-60 DEG C of breast
At a temperature of change, using high-speed shearing machine shear agitation emulsifying agent, shearing rotating speed is in 5000-6000rpm, after emulsifying agent is well mixed
Synthetic guttapercha glue is added, continues stirring under shearing rotating speed 10000-11000rpm rotating speed until homogenizing completion, latex
Average grain diameter is 430-550nm.
Further, primary emulsion is anionic emulsifier, and assistant for emulsifying agent is nonionic emulsifier, and stabilizer is selected from poly-
One or more in PAA, polyacrylic acid potassium, polyethylene glycol or polyvinyl alcohol.
Further, the anionic emulsifier is selected from alkylbenzenesulfonate, alkyl sulphur of the alkyl carbon number between 6-22
One or more of anionic emulsifier in hydrochlorate, alkylnaphthalene sulfonate, alkyl sulfate；Be more highly preferred to, it is described it is cloudy from
One or more of the subtype emulsifying agent in neopelex, disproportionated rosin acid potassium, potassium oleate.
Further, the nonionic emulsifier is selected generally from aliphatic alcohol polyethenoxy of the alkyl carbon number between 6-22
One or more of nonionic emulsifier in ether, aliphatic amine polyoxyethylene ether, alkylbenzene APEO；Nonionic emulsifies
Agent can be selected from sapn (SPAN) serial (AEO), tween (TWEEN) serial (AEO),
One or more of nonionic emulsifier in peregal series (AEO), especially sorbester p17, polysorbate60
In one or more；It is more highly preferred to, the stabilizer preferably is selected from PEG-4000, PEG-4000, polypropylene
One or more in sour sodium.
Synthetic guttapercha latex after emulsification, is specifically pumped into evaporating kettle by the step (1.3), opens stirring, first
Choosing carries out air-distillation, opens vacuum system after distillate drip speed is slack-off, starts to be evaporated under reduced pressure, when distillate drip speed is bright
After showing slack-off, terminate solvent removal, synthetic guttapercha dilute latex is made；Air-distillation temperature is 70-85 DEG C, vacuum distillation temperature
For 70-85 DEG C, vacuum is gauge pressure 0.05-0.07Mpa, and vapo(u)rizing temperature is higher than the boiling point 78-80 of synthetic guttapercha glue solvent
DEG C, mixing speed is between 200--400rpm scopes.
In the step (1.4.), the synthetic guttapercha dilute latex after desolvation is carried out using ultracentrifugal method
Concentration, the synthetic guttapercha dilute latex after desolvation is put into supercentrifuge, sets centrifugal rotational speed as 6000-
8000rpm, centrifugation time 1-10min, open supercentrifuge and start to be concentrated into centrifugation and terminate, final finished synthetic guttapercha
The solid content mass percent of latex is between 40-80%；The Best Times of centrifugation are 2-6min.
The advantageous effects of the present invention are as follows：A certain amount of synthetic guttapercha micelle is dissolved using good solvent, and synthesis is made
Gutta-percha glue, directly emulsified, desolvation and concentration, the technological process it is succinct；The present invention makes synthetic guttapercha
The dispersed and interface interaction of synthetic guttapercha and filler is realized after latex in the form of wet method refining glue, makes to be prepared
Synthetic guttapercha breast compound with regular structure, easily crystallization, be hard material at normal temperatures, when unvulcanized, can make as thermoplastic
With being usually used in protecting ware for sports and artificial limb set, after vulcanization, can be used as thermoelastic material, be usually used in shape-memory material, simultaneously
It can also be used with other rubber and plastic blend as elastomeric material.
Embodiment
The invention discloses a kind of preparation method of synthetic guttapercha breast, those skilled in the art can be used for reference in this paper
Hold, be suitably modified technological parameter realization.In particular, all similar replacements and change are to those skilled in the art
For be it will be apparent that they are considered as being included among the present invention.The method of the present invention and application are by preferable
Embodiment is described, related personnel substantially can not depart from present invention, in spirit and scope to side as described herein
Method and application are modified or suitably changed with combining, to realize and using the technology of the present invention.
Embodiment 1
The preparation of synthetic guttapercha glue sequentially adds quantitative hexamethylene and synthetic guttapercha in the reactor, and opening is stirred
Mix, solution temperature is 75 DEG C, and dissolution time is 8 hours；
When the emulsification emulsifier concentration of synthetic guttapercha glue is 7.0% (aqueous phase mass fraction), add in container
Enter a small amount of deionized water, the mass ratio of primary emulsion and assistant for emulsifying agent is 2.0, and it is 25% to sequentially add mass percent concentration
Primary emulsion disproportionated rosin acid potassium 16.8g (25% × 16.8=4.2g) and 2.1g assistant for emulsifying agents neopelex,
0.09g PEG-4000s are adjusted pH 12 or so as stabilizer, using KOH, add deionized water so that aqueous phase matter
Amount reaches 90g, and now oil-water ratio is 1.0；At a temperature of 60 DEG C, using the above-mentioned emulsification prepared of high-speed shearing machine shear agitation
Agent, rotating speed control in 5000rpm, after emulsifying agent is well mixed, are slowly added to prepared synthetic guttapercha glue, add speed
To ensure that emulsification is uniformly advisable, 10min is kept to ensure to have emulsified under this rotating speed after the completion of the charging of synthetic guttapercha glue
Entirely, then by adjustment of rotational speed 8000rpm or so is arrived, is homogenized closing high-speed cutter after 5min, the emulsion process of glue is completed.To glue
Milk particle footpath is detected, and latex particle size is 279nm under the conditions of the present embodiment.
Conjunction of the solvent removal of synthetic guttapercha latex first at 80 DEG C by the solvent of the above-mentioned preparations of 100ml for hexamethylene
It is put into gutta-percha latex in evaporating kettles of the 500ml with magnetic agitation, carries out air-distillation, mixing speed control exists
350rpm or so, after distillate drip speed is obvious slack-off, most of solvent is distilled out of, and now opens vacuum system, starts to subtract
The temperature that pressure distillation is evaporated under reduced pressure is 70 DEG C, and system is depressurized to gauge pressure 0.05MPa, mixing speed 400rpm, when steaming drop
Flow velocity it is obvious it is slack-off after, terminate solvent removal, synthetic guttapercha dilute latex be made.
Obtained dilute latex is put into supercentrifuge by the concentration of synthetic guttapercha breast, and centrifugal rotational speed is adjusted to
8000rpm or so, start high speed centrifugation concentration, centrifugation time 2min, the solid content of gained synthetic guttapercha concentrated latex is about
For 80%.
Embodiment 2
The preparation of synthetic guttapercha glue sequentially adds quantitative pentane and synthetic guttapercha in the reactor, and opening is stirred
Mix, solution temperature is 70 DEG C, and dissolution time is 8 hours；
When the emulsification emulsifier concentration of synthetic guttapercha glue is 5.0% (aqueous phase mass fraction), add in container
Enter a small amount of deionized water, the mass ratio of primary emulsion and assistant for emulsifying agent is 3.0, and it is 25% to sequentially add mass percent concentration
Disproportionated rosin acid potassium 10g (25% × 10=2.25g) and neopelex 1.25g are as primary emulsion and 1.25g
Assistant for emulsifying agent alkylbenzene APEO, 0.1g Sodium Polyacrylates are adjusted pH 12 or so as stabilizer, using KOH, then
Deionized water is added so that aqueous phase quality reaches 100g, now oil-water ratio is 0.8.At a temperature of 60 DEG C, using high-speed shearing machine
The above-mentioned emulsifying agent prepared of shear agitation, rotating speed are controlled in 6000rpm, after emulsifying agent is well mixed, are slowly added to prepared
Synthetic guttapercha glue, add speed with ensure emulsification be uniformly advisable, when synthetic guttapercha glue feed after the completion of in this turn
Speed is lower to keep 10min to ensure that emulsification is complete, then by adjustment of rotational speed to 11000rpm, closing high-speed cutter after homogenizing 5min,
The emulsion process of glue is completed.Latex particle size is detected, latex particle size is 430nm under the conditions of the present embodiment.
Conjunction of the solvent removal of synthetic guttapercha latex first at 85 DEG C by the solvent of the above-mentioned preparations of 100ml for hexamethylene
It is put into gutta-percha latex in evaporating kettles of the 500ml with magnetic agitation, carries out air-distillation, mixing speed control exists
350rpm or so, after distillate drip speed is obvious slack-off, most of solvent is distilled out of, and now opens vacuum system, starts to subtract
Pressure distillation, the temperature of vacuum distillation are 85 DEG C, and system is depressurized to gauge pressure 0.07MPa, mixing speed 200rpm, when steaming drop
Flow velocity it is obvious it is slack-off after, terminate solvent removal, synthetic guttapercha dilute latex be made.
Obtained dilute latex is put into supercentrifuge by the concentration of synthetic guttapercha breast, and centrifugal rotational speed is adjusted to
6000rpm or so, start high speed centrifugation concentration, centrifugation time 10min, the solid content of gained synthetic guttapercha concentrated latex is about
For 60%.
Embodiment 3
The preparation of synthetic guttapercha glue sequentially adds quantitative n-hexane and synthetic guttapercha in the reactor, and opening is stirred
Mix, solution temperature is 80 DEG C, and dissolution time is 8 hours；
When the emulsification emulsifier concentration of synthetic guttapercha glue is 3.0% (aqueous phase mass fraction), add in container
Enter a small amount of deionized water, the mass ratio of primary emulsion and assistant for emulsifying agent is 1.0, and it is 25% to sequentially add mass percent concentration
Disproportionated rosin acid potassium 7.2g (25% × 7.2=1.8g) as primary emulsion and 1.8g aliphatic amine polyoxyethylene classes assistant for emulsifying agent,
0.12g PEG-4000s and PEG-4000 are adjusted pH 12 or so as stabilizer, using KOH, are added
Ionized water is so that aqueous phase quality reaches 120g, and now oil-water ratio is 0.5.At a temperature of 60 DEG C, stirred using high-speed shearing machine shearing
The above-mentioned emulsifying agent prepared is mixed, rotating speed is controlled in 5000rpm-6000rpm or so, after emulsifying agent is well mixed, is slowly added to
Prepared synthetic guttapercha glue, speed is added to ensure that emulsification is uniformly advisable, after the completion of the charging of synthetic guttapercha glue
10min is kept under this rotating speed to ensure that emulsification is complete, then adjustment of rotational speed is arrived into 10000rpm or so, closing is high after being homogenized 5min
Fast cutter, the emulsion process of glue are completed.Latex particle size is detected, latex particle size is 550nm under the conditions of the present embodiment.
Conjunction of the solvent removal of synthetic guttapercha latex first at 82 DEG C by the solvent of the above-mentioned preparations of 100ml for hexamethylene
It is put into gutta-percha latex in evaporating kettles of the 500ml with magnetic agitation, carries out air-distillation, mixing speed control exists
350rpm or so, after distillate drip speed is obvious slack-off, most of solvent is distilled out of, and now opens vacuum system, starts to subtract
Pressure distillation, the temperature of vacuum distillation are 78 DEG C, and system is depressurized to gauge pressure 0.06MPa, mixing speed 300rpm, when steaming drop
Flow velocity it is obvious it is slack-off after, terminate solvent removal, synthetic guttapercha dilute latex be made.
Obtained dilute latex is put into supercentrifuge by the concentration of synthetic guttapercha breast, and centrifugal rotational speed is adjusted to
7000rpm or so, start high speed centrifugation concentration, centrifugation time 6min, the solid content of gained synthetic guttapercha concentrated latex is about
For 40%.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of synthetic guttapercha breast, it is characterised in that comprise the following steps：
(1.1) using nonpolar saturated alkane as solvent, synthetic guttapercha is added, opens stirring, rising temperature for dissolving obtains synthesizing the bark of eucommia
Glue；
(1.2) synthetic guttapercha liquid is emulsified with emulsifier aqueous solution by high speed shear method；
(1.3) the synthetic guttapercha breast after emulsification is distilled, desolvation obtains synthetic guttapercha dilute latex；
(1.4) the synthetic guttapercha dilute latex after desolvation is concentrated using ultracentrifugal method, obtains 40-80%
The finished product synthetic guttapercha breast of solid content.
2. preparation method as claimed in claim 1, it is characterised in that in the step (1.1), the temperature of rising temperature for dissolving is
70-80 DEG C, dissolution time is 8 hours；Nonpolar saturated alkane solvent is selected from hexamethylene, n-hexane, pentamethylene or pentane.
3. preparation method as claimed in claim 1, it is characterised in that in the step (1.2), emulsifying agent by primary emulsion,
Assistant for emulsifying agent and stabilizer composition, add deionized water in the glue emulsifier with high shear agitation, sequentially add master
Emulsifying agent, assistant for emulsifying agent and stabilizer, using alkali hydroxide come to adjust the pH value of emulsion be 10-12, deionization is added again
Water is so that profit mass ratio reaches 0.5-1.0, and the mass ratio of primary emulsion and assistant for emulsifying agent is 1.0-3.0, the dosage of emulsifying agent
For the 3.0-7.0% of aqueous phase mass percent, the dosage of stabilizer is the 0.01-0.05% of aqueous phase mass percent；In 40-60
DEG C emulsifying temperature under, using high-speed shearing machine shear agitation emulsifying agent, shearing rotating speed is in 5000-6000rpm, emulsifying agent mixing
It is uniformly rear to add synthetic guttapercha liquid, continue to stir under shearing rotating speed 10000-11000rpm rotating speed up to homogenizing completion,
Latex average grain diameter is 430-550nm.
4. preparation method as claimed in claim 3, it is characterised in that primary emulsion is anionic emulsifier, assistant for emulsifying agent
For nonionic emulsifier, one kind in Sodium Polyacrylate, polyacrylic acid potassium, polyethylene glycol or polyvinyl alcohol of stabilizer or
It is several.
5. preparation method as claimed in claim 4, it is characterised in that the anionic emulsifier is selected from alkyl carbon number in 6-
One or more of anionics in alkylbenzenesulfonate, alkylsulfonate, alkylnaphthalene sulfonate, alkyl sulfate between 22
Emulsifying agent, the nonionic emulsifier are selected generally from AEO, fatty amine of the alkyl carbon number between 6-22
One or more of nonionic emulsifier in APEO, alkylbenzene APEO.
6. preparation method as claimed in claim 5, it is characterised in that the anionic emulsifier is selected from detergent alkylate sulphur
One or more in sour sodium, disproportionated rosin acid potassium, potassium oleate, the stabilizer preferably are selected from PEG-4000, poly- second two
One or more in alcohol -4000, Sodium Polyacrylate.
7. preparation method as claimed in claim 1, it is characterised in that the step (1.3), specifically by the synthesis after emulsification
Bark of eucommia latex is pumped into evaporating kettle, and first choice carries out air-distillation, is opened vacuum system after distillate drip speed is slack-off, is started to subtract
Pressure distillation, after distillate drip speed is obvious slack-off, terminates solvent removal, synthetic guttapercha dilute latex is made；Air-distillation temperature
Spend for 70-85 DEG C, vacuum distillation temperature is 70-85 DEG C, and vacuum is gauge pressure 0.05-0.07Mpa, and vapo(u)rizing temperature is shut out higher than synthesis
78-80 DEG C of the boiling point of secondary glue solvent, mixing speed 200-400rpm.
8. preparation method as claimed in claim 1, it is characterised in that in the step (1.4.), using ultracentrifugal side
Method is concentrated to the synthetic guttapercha dilute latex after desolvation, and the synthetic guttapercha dilute latex after desolvation is put into height
In fast centrifuge, centrifugal rotational speed is set as 6000-8000rpm, and centrifugation time 1-10min, opening supercentrifuge starts dense
It is reduced to centrifugation to terminate, the solid content mass percent of final finished synthetic guttapercha breast is between 40-80%.
9. preparation method as claimed in claim 8, it is characterised in that centrifugation time 2-6min.
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Cited By (8)
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| CN108424530A (en) * | 2018-03-14 | 2018-08-21 | 中国化工株洲橡胶研究设计院有限公司 | A kind of preparation method of Cortex Eucommiae latex |
| CN109553379A (en) * | 2018-12-11 | 2019-04-02 | 公安部四川消防研究所 | Intumescent fire retardant module and its processing method |
| CN110423361A (en) * | 2019-08-20 | 2019-11-08 | 贵州大学 | A kind of natural gutta-percha lotion |
| CN110437510A (en) * | 2019-07-31 | 2019-11-12 | 中国化工株洲橡胶研究设计院有限公司 | A kind of gutta-percha/natural emulsion sponge product and preparation method thereof |
| CN110862466A (en) * | 2019-12-02 | 2020-03-06 | 中国化工株洲橡胶研究设计院有限公司 | Concentration method of low-concentration eucommia ulmoides latex |
| CN112175203A (en) * | 2020-11-04 | 2021-01-05 | 中国化工株洲橡胶研究设计院有限公司 | Preparation method of natural gutta-percha emulsion |
| CN112457503A (en) * | 2020-11-26 | 2021-03-09 | 中国化工株洲橡胶研究设计院有限公司 | Preparation method of epoxidized eucommia ulmoides latex |
| CN112513147A (en) * | 2018-08-29 | 2021-03-16 | 日本瑞翁株式会社 | Method for producing polymer latex |
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| US3250737A (en) * | 1961-08-21 | 1966-05-10 | Shell Oil Co | Preparation of concentrated latices by alternately flashing and centrifuging |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424530A (en) * | 2018-03-14 | 2018-08-21 | 中国化工株洲橡胶研究设计院有限公司 | A kind of preparation method of Cortex Eucommiae latex |
| CN112513147A (en) * | 2018-08-29 | 2021-03-16 | 日本瑞翁株式会社 | Method for producing polymer latex |
| CN109553379A (en) * | 2018-12-11 | 2019-04-02 | 公安部四川消防研究所 | Intumescent fire retardant module and its processing method |
| CN109553379B (en) * | 2018-12-11 | 2021-04-30 | 公安部四川消防研究所 | Expansion type fire-retardant module and processing method thereof |
| CN110437510A (en) * | 2019-07-31 | 2019-11-12 | 中国化工株洲橡胶研究设计院有限公司 | A kind of gutta-percha/natural emulsion sponge product and preparation method thereof |
| CN110437510B (en) * | 2019-07-31 | 2022-02-25 | 中国化工株洲橡胶研究设计院有限公司 | Gutta-percha/natural latex sponge product and preparation method thereof |
| CN110423361A (en) * | 2019-08-20 | 2019-11-08 | 贵州大学 | A kind of natural gutta-percha lotion |
| CN110862466A (en) * | 2019-12-02 | 2020-03-06 | 中国化工株洲橡胶研究设计院有限公司 | Concentration method of low-concentration eucommia ulmoides latex |
| CN110862466B (en) * | 2019-12-02 | 2022-05-20 | 中国化工株洲橡胶研究设计院有限公司 | Concentration method of low-concentration eucommia ulmoides latex |
| CN112175203A (en) * | 2020-11-04 | 2021-01-05 | 中国化工株洲橡胶研究设计院有限公司 | Preparation method of natural gutta-percha emulsion |
| CN112175203B (en) * | 2020-11-04 | 2022-11-22 | 中国化工株洲橡胶研究设计院有限公司 | Preparation method of natural gutta-percha emulsion |
| CN112457503A (en) * | 2020-11-26 | 2021-03-09 | 中国化工株洲橡胶研究设计院有限公司 | Preparation method of epoxidized eucommia ulmoides latex |
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