CN101475785A - Binder and preparation thereof - Google Patents
Binder and preparation thereof Download PDFInfo
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- CN101475785A CN101475785A CNA2009100009151A CN200910000915A CN101475785A CN 101475785 A CN101475785 A CN 101475785A CN A2009100009151 A CNA2009100009151 A CN A2009100009151A CN 200910000915 A CN200910000915 A CN 200910000915A CN 101475785 A CN101475785 A CN 101475785A
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- Prior art keywords
- binding agent
- latex
- pva
- polyvinyl acetate
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- 239000011230 binding agent Substances 0.000 title claims description 87
- 238000002360 preparation method Methods 0.000 title claims description 39
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 56
- 239000004816 latex Substances 0.000 claims abstract description 53
- 229920000126 latex Polymers 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 43
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 27
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 150000001733 carboxylic acid esters Chemical class 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 45
- 239000000203 mixture Substances 0.000 claims description 40
- 239000000178 monomer Substances 0.000 claims description 28
- 239000003999 initiator Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000004160 Ammonium persulphate Substances 0.000 claims description 17
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 17
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 125000002252 acyl group Chemical group 0.000 claims description 16
- 238000005502 peroxidation Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 239000004927 clay Substances 0.000 claims description 11
- 239000005995 Aluminium silicate Substances 0.000 claims description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims description 8
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 8
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 13
- 239000000853 adhesive Substances 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 3
- 229920002689 polyvinyl acetate Polymers 0.000 abstract 3
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000011056 performance test Methods 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000004576 sand Substances 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 125000005395 methacrylic acid group Chemical group 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 150000003460 sulfonic acids Chemical class 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000000655 anti-hydrolysis Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000009973 maize Nutrition 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003027 oil sand Substances 0.000 description 1
- 239000001254 oxidized starch Substances 0.000 description 1
- 235000013808 oxidized starch Nutrition 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Polymerisation Methods In General (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to an adhesive. The adhesive mainly comprises polyvinyl acetate latex and refractory powder; the adhesive is used as a whole; the weight portion of the polyvinyl acetate latex is between 35 and 65; the weight portion of the refractory powder is between 40 and 70; vinyl acetate and carboxylic ester in an alcoholic solvent are subjected to evocation and polymerization through a chemical evocating agent to form the polyvinyl acetate latex; and the viscosity of the adhesive is between 800 and 2,000 centipoises. The invention also provides a method for preparing the adhesive. The prepared adhesive has the advantages of high strength, hydrolytic resistance, rapid curing speed, and the like.
Description
Technical field
The invention belongs to the binding agent field, relate to a kind of binding agent that is used for casting field specifically.
Background technology
At present, the polyvinyl acetate (PVA) latex is a kind of emulsion adhesive commonly used, have that curing speed is fast, cohesive strength is high, cost is low, eco-friendly advantage, be widely used in the many aspects of casting, building, daily life, as be used for the process that sand mold is repaired fast, therefore need binding agent to have the performance that curing speed is fast, cohesive strength is high.But as can be seen from the vinyl acetate molecular structural formula, it has the double properties of alkene and ester class concurrently, generate in the process of polyvinyl acetate (PVA) latex in polyreaction, Raolical polymerizable and basic hydrolysis can take place, cause defectives such as this class binding agent water tolerance and winter hardiness difference, and normally used polyvinyl acetate (PVA) emulsion adopts water-soluble system, causes this class adhesive cures speed slower, makes its application be very limited.
As 38 pages of adhesive property researchs that disclose Sumstar 190 and polyvinyl acetate (PVA) latex co-mixing system of Chinese document " fine chemistry industry " nineteen ninety-five the 12nd volume, prepare maize oxidized starch liquid and polyvinyl acetate (PVA) latex at first respectively, wherein the preparation process of Sumstar 190 is: after order adds hydrogen peroxide, ferrous sulfate, sodium hydroxide solution, borax in W-Gum, add terminator at last and stir and can obtain Sumstar 190; The preparation process of polyvinyl acetate (PVA) latex is: with polyvinyl alcohol and distilled water mixing post-heating, and order adds emulsifying agent and conditioning agent, add vinyl acetate between to for plastic and ammonium persulphate again, add an amount of softening agent and an amount of stablizer at last, can obtain the polyvinyl acetate (PVA) latex after stirring.The prior art is mixed the polyvinyl acetate (PVA) latex of preparing according to a certain percentage with Sumstar 190, the polyvinyl acetate (PVA) latex is carried out modification to overcome defectives such as polyvinyl acetate (PVA) emulsion binder water tolerance and winter hardiness difference, through shearing resistance and water-fast test, prove that the polyvinyl acetate (PVA) latex of blend has better cohesive strength and water resistance.But still there is following defective in the prior art: (1) can be found out from empirical value, the tackiness agent of the prior art preparation is in shearing test, solidified 48 hours under the room temperature, the cohesive strength of tackiness agent constantly increase and the shearing resistance when recording 48 hours only for about 3MPa, as seen prior art can not reach quick-setting purpose, and cohesive strength is unsatisfactory.(2) in the prior art in the preparation process of polyvinyl acetate (PVA) latex, only improve the viscosity and the cohesive strength of polyvinyl acetate (PVA) latex by the content that increases polyvinyl alcohol, because chemical reagent prices such as polyvinyl alcohol are relatively costly, in industrial mass production, if will obtain the binding agent of high bond strength, just need a large amount of polyvinyl alcohol, cause production cost to increase greatly.In addition, if want to regulate the final strength of binding agent, just need be before polymerization process each proportion of raw materials of accurate calculation, might cause the bigger variation of product cohesive strength generation because of trickle variation, and the cohesive strength that can't regulate product once more, cause the waste of manpower and materials.
Summary of the invention
For this reason, technical problem to be solved by this invention is: overcome the shortcoming that adhesive solidification speed is slow in the prior art, production cost is higher.
For solving the problems of the technologies described above, the invention provides a kind of binding agent, described binding agent comprises and mainly comprises polyvinyl acetate (PVA) latex and refractory powder, with described binding agent is an integral body, the parts by weight of described polyvinyl acetate (PVA) latex are 35-65 part, the parts by weight of described refractory powder are 40-70 part, and described polyvinyl acetate (PVA) latex draws agent initiated polymerization by chemistry by vinyl acetate and carboxylicesters and forms in alcoholic solvent; Viscosity is the 800-2000 centipoise.
As a whole with described polyvinyl acetate (PVA) latex, each raw materials in part by weight that polymerization forms described polyvinyl acetate (PVA) latex is respectively:
Vinyl acetate 20-50 part;
Carboxylicesters 5-25 part;
Alcoholic solvent 10-35 part;
Initiator 0.03-1.3 part.
Described initiator is ammonium persulphate and/or peroxidation two acyls.
Described initiator is the mixture of ammonium persulphate and peroxidation two acyls, and both weight ratios are 1:1-2:1.
Described carboxylicesters is one or more in acrylate, methacrylic ester, Isooctyl acrylate monomer, butyl acrylate, vinyl acetic monomer, the N-BUTYL ACETATE.
Described alcoholic solvent is methyl alcohol and/or ethanol.
Described refractory powder is one or more in talcum powder, silica powder, kaolin, clay, the bauxitic clay.
The preparation method of described binding agent comprises the steps:
A) polymerization procedure: earlier initiator is dissolved in the alcoholic solvent and treats to form the initiator alcoholic solution, again with vinyl acetate, carboxylicesters mixes to form mix monomer, the described mix monomer of 50-80% (weight) is added in the reactor, constantly slowly add the described initiator alcoholic solution of part under the condition of stirring for the first time, after polyreaction 0.5-2.5 hour, all join the described mix monomer of remaining 20-50% (weight) in the described reactor slowly again, and in adding the process of described residue mix monomer, slowly repeatedly add remaining described initiator alcoholic solution for the second time, temperature is controlled at 55-75 ℃ in the whole polymerization process, stop polyreaction when mixture viscosity at room temperature is the 500-1000 centipoise in reactor, and obtain polymerisate;
B) dilution step: in described polymerisate, add alcoholic solvent, obtain the polyvinyl acetate (PVA) latex after fully stirring;
C) blending dispersion step: under stirring condition, slowly repeatedly add refractory powder in the described polyvinyl acetate (PVA) latex that in polymerization procedure, obtains, stop when at room temperature viscosity is the 4000-10000 centipoise adding until mixture, and finally obtain described binding agent, wherein, with described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 35-65 part, and the parts by weight of described refractory powder are 40-70 part.
Described initiator is the mixture of ammonium persulphate and peroxidation two acyls, and both weight ratios are 1:1-2:1.
Described carboxylicesters is one or more in acrylate, methacrylic ester, Isooctyl acrylate monomer, butyl acrylate, vinyl acetic monomer, the N-BUTYL ACETATE; Described alcoholic solvent is methyl alcohol and/or ethanol; Described refractory powder is one or more in talcum powder, silica powder, kaolin, clay, the bauxitic clay.
Compared with prior art the present invention has the following advantages:
(1) in experiment, finds, the polyvinyl acetate (PVA) latex mainly adopts water-soluble system in the prior art, it is bigger to cause containing water gaging in the binding agent, and because there are the characteristics of water tolerance and winter hardiness difference in polyvinyl acetate (PVA) self, so the binding agent cohesive strength is not high, the curing speed of the tackiness agent under the normal temperature condition of water-content higher meeting reduction the simultaneously.And adopt alcohols among the present invention in the adhesive preparation process as solvent, because alcohols has the curing speed and the cohesive strength height that can improve binding agent in the good characteristics of volatile performance greatly.
(2) binding agent of the present invention can reach the purpose of regulated at will binding agent cohesive strength according to actual needs by regulating the ratio of polyvinyl acetate (PVA) latex and refractory powder.In addition, because the control of the cohesive strength of the binding agent of preparing among the present invention can be regulated when adding refractory powder once more, even the intensity of preparation polyvinyl acetate (PVA) latex is too small or excessive, also can remedy, make the cohesive strength of final binding agent be more prone to control by the add-on of regulating refractory powder.Simultaneously, because binding agent is made of jointly higher polyvinyl acetate (PVA) latex of cost and cheap refractory powder,, make that the cost of binding agent reduces greatly among the present invention than existing pure chemistry binding agent.
Embodiment
Embodiment 1
The preparation process of binding agent comprises:
A) rectification step: earlier whole vinyl acetate 20-50 parts are squeezed into stirring tank, 60-70 ℃ of temperature rising reflux wherein distillates and is that vinyl acetate, still go out to be high boiling material, comprising a large amount of stoppers.Return time is 2-4 hour, and return velocity obviously reduces or temperature in the kettle obviously raises and during more than or equal to 85 ℃, rectification working process finishes.
B) polymerization procedure: under 40-60 ℃, with ammonium persulphate and the dissolving of peroxidation two acyls, it is stand-by to form the initiator alcoholic solution with methyl alcohol, and wherein, the ratio of weight and number of ammonium persulphate and peroxidation two acyls is 1:1.
With vinyl acetate; vinyl acetic monomer; acrylate; methacrylic ester and Isooctyl acrylate monomer mix to form mix monomer; the described mix monomer adding of 80% (weight) is had mechanical stirring; in the reactor of condenser and nitrogen protection pipe; the control stirring velocity be 50-70 rev/min and with steam heating to 65-75 ℃ after 5-25 minute; the described initiator alcoholic solution that adds for the first time 60% (weight); the beginning initiated polymerization; after the polyreaction 2.5 hours; all join the described mix monomer of remaining 20% (weight) in the described reactor slowly again; strict control feed rate added remaining mix monomer in 60 minutes.In the process that adds described residue mix monomer, be divided into the remaining described initiator alcoholic solution of twice adding for the second time lentamente.Temperature of reaction is controlled at 65-75 ℃ and timing sampling always in the polymerization process, stops polyreaction when mixture viscosity at room temperature is 1000 centipoises to reactor, and obtains polymerisate.
B) dilution step: make the temperature of the described polymerisate that polymerization generates in the reactor reduce to 55 ℃, slowly add methanol solvate, the reinforced 10-40 minute process time spent, fully stirred again 10-30 minute behind reinforced the finishing, finally obtain the polyvinyl acetate (PVA) latex.
C) blending dispersion step: under stirring condition, the mixture that slowly repeatedly adds refractory powder talcum powder, silica powder, clay in the described polyvinyl acetate (PVA) latex that in polymerization procedure, obtains, the control rotating speed is 90-120 rev/min, the reinforced 30-60 minute process time spent, behind reinforced the finishing again normal temperature fully stirred 1-2 hour, stop when at room temperature viscosity is 10000 centipoises adding until mixture, and finally obtain described binding agent A1.
Wherein, as a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
20 parts of vinyl acetates;
5 parts of vinyl acetic monomers;
3 parts of acrylate;
2 parts of methacrylic esters;
1 part of Isooctyl acrylate monomer;
10 parts of methyl alcohol;
0.03 part in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
20 parts of talcum powder;
20 parts of silica powders;
0.4 part of clay.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 35 parts, and the parts by weight of described refractory powder are 40 parts.
The The performance test results that present embodiment prepares binding agent S1 sees Table 1.
In the polymerization procedure of preparation binding agent step, need to prove: the vinyl acetate that uses in (1) present embodiment is the commercially available prod, in order to guarantee that autohemagglutination does not during preservation take place for it or other cause the rotten reaction of vinyl acetate, in product, add additives such as stopper usually.So in the production technique of preparation binding agent, be not subjected to the influence of these additives, generally need to carry out in the present embodiment rectification step in the preparation binding agent step to remove the additives such as stopper in the vinyl acetate in order to guarantee polyreaction.Certainly, if do not add any additives in the product that uses, then prepare in the step of binding agent and can not carry out rectification step.(2) because the polymerization reaction system of preparation polyvinyl acetate (PVA) latex need could cause in inert atmosphere and carry out polyreaction, so need to feed rare gas element in the reactor so that inert atmosphere to be provided, rare gas element can be nitrogen, argon gas, helium etc.(3) initiator must add in gradation, reason is if once all initiator is added, can cause the initial reaction of system very fast, speed of response is difficult to control, and the later stage speed of response reduces, and reaction again can be not thorough, and it is inhomogeneous speed of response promptly to occur, molecular weight is not of uniform size, the phenomenon that quality stability is too poor.Because above-mentioned (1), (2) two technology contents are well known to those skilled in the art, and are not key protection points of the present invention, so be not described further.
The purpose of adding refractory powder is to regulate described polyvinyl acetate (PVA) latex in the binding agent in the present embodiment viscosity and intensity, promptly regulate the proportioning of polyvinyl acetate (PVA) latex and refractory powder, thereby realize regulating the purpose of the whole cohesive strength of binding agent according to user's actual needs.On the other hand, because refractory powder cheap, thereby reduce the cost of preparation binding agent greatly.
By preparation process as can be seen, the water-content in the binding agent of the present invention is very low, mainly adopts pure solution to be, can improve adhesive cures speed on the one hand; On the other hand, can reduce the destruction of tax molecule, improve the environment tolerance of binding agent the binding agent internal network.
Embodiment 2
In the present embodiment, the preparation process of binding agent is identical with embodiment 1, and only the parts by weight to preparation binding agent desired raw material change.
As a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
50 parts of vinyl acetates;
5 parts of vinyl acetic monomers;
10 parts of acrylate;
5 parts of methacrylic esters;
5 parts of Isooctyl acrylate monomers;
35 parts of methyl alcohol;
1.3 parts in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
30 parts of talcum powder;
35 parts of silica powders;
4 parts of clays.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 65 parts, and the parts by weight of described refractory powder are 70 parts.
The The performance test results that present embodiment prepares binding agent S2 sees Table 1.
Embodiment 3
In the present embodiment, the preparation process of binding agent is identical with embodiment 1, and only the parts by weight to preparation binding agent desired raw material change.
In the binding agent,
As a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
25 parts of vinyl acetates;
3 parts of vinyl acetic monomers;
2 parts of acrylate;
1 part of methacrylic ester;
1 part of Isooctyl acrylate monomer;
20 parts of methyl alcohol;
0.5 part in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
30 parts of talcum powder;
20 parts of silica powders;
2 parts of clays.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 50 parts, and the parts by weight of described refractory powder are 55 parts.
The The performance test results that present embodiment prepares binding agent S3 sees Table 1.
Embodiment 4
The preparation process of binding agent comprises in the present embodiment:
A) rectification step: earlier whole vinyl acetate 20-50 parts are squeezed into stirring tank, 60-70 ℃ of temperature rising reflux wherein distillates and is that vinyl acetate, still go out to be high boiling material, comprising a large amount of stoppers.Return time is 2-4 hour, and return velocity obviously reduces or temperature in the kettle obviously raises and during more than or equal to 85 ℃, rectification working process finishes.
B) polymerization procedure: under 40-60 ℃, with methyl alcohol and alcoholic acid mixed solution ammonium persulphate and peroxidation two acyls are dissolved, it is stand-by to form the initiator alcoholic solution, and wherein, the ratio of weight and number of ammonium persulphate and peroxidation two acyls is 2:1.
With vinyl acetate; acrylate; Isooctyl acrylate monomer mixes to form mix monomer; the described mix monomer adding of 50% (weight) is had mechanical stirring; in the reactor of condenser and nitrogen protection pipe; the control stirring velocity be 70-90 rev/min and with steam heating to 55-65 ℃ after 5-25 minute; the described initiator alcoholic solution that adds for the first time 60% (weight); the beginning initiated polymerization; after the polyreaction 0.5 hour; all join the described mix monomer of remaining 50% (weight) in the described reactor slowly again; strict control feed rate added remaining mix monomer in 90 minutes.In the process that adds described residue mix monomer, be divided into the remaining described initiator alcoholic solution of twice adding for the second time lentamente.Temperature of reaction is controlled at 55-65 ℃ and timing sampling always in the polymerization process, stops polyreaction when mixture viscosity at room temperature is 500 centipoises to reactor, and obtains polymerisate.
B) dilution step: make the temperature of the described polymerisate that polymerization generates in the reactor reduce to room temperature ℃, slowly add methyl alcohol and ethanol mixed solvent, the reinforced 10-40 minute process time spent, fully stirred again 10-30 minute behind reinforced the finishing, finally obtain the polyvinyl acetate (PVA) latex.
C) blending dispersion step: under stirring condition, the mixture that slowly repeatedly adds refractory powder kaolin and bauxitic clay in the described polyvinyl acetate (PVA) latex that in polymerization procedure, obtains, the control rotating speed is 90-120 rev/min, the reinforced 30-60 minute process time spent, behind reinforced the finishing again normal temperature fully stirred 1-2 hour, stop when at room temperature viscosity is 4000 centipoises adding until mixture, and finally obtain described binding agent A5.
Wherein, as a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
20 parts of vinyl acetates;
5 parts of N-BUTYL ACETATEs;
5 parts of acrylate;
1 part of Isooctyl acrylate monomer;
10 parts of methyl alcohol and ethanol mixed solvent;
0.03 part in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
20 parts of kaolin;
21 parts of bauxitic clays.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 35 parts, and the parts by weight of described refractory powder are 40 parts.
The The performance test results that present embodiment prepares binding agent S4 sees Table 1.
Embodiment 5
In the present embodiment, the preparation process of binding agent is identical with embodiment 4, and only the parts by weight to preparation binding agent desired raw material change.
In the binding agent,
As a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
50 parts of vinyl acetates;
10 parts of N-BUTYL ACETATEs;
10 parts of acrylate;
5 parts of Isooctyl acrylate monomers;
35 parts of methyl alcohol and ethanol mixed solvent;
1.3 parts in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
30 parts of kaolin;
40 parts of bauxitic clays.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 65 parts, and the parts by weight of described refractory powder are 70 parts.
The The performance test results that present embodiment prepares binding agent S5 sees Table 1.
Embodiment 6
In the present embodiment, the preparation process of binding agent is identical with embodiment 5, and only the parts by weight to preparation binding agent desired raw material change.
In the binding agent,
As a whole with described polyvinyl acetate (PVA) latex, each required in preparation process raw materials in part by weight is respectively:
25 parts of vinyl acetates;
3 parts of N-BUTYL ACETATEs;
2 parts of acrylate;
1 part of Isooctyl acrylate monomer;
20 parts of methyl alcohol and ethanol mixed solvent;
0.5 part in ammonium persulphate and peroxidation two acyl mixtures (ratio of weight and number is 1:1);
Do with refractory powder as a whole, wherein:
30 parts of kaolin;
22 parts of bauxitic clays.
With described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 50 parts, and the parts by weight of described refractory powder are 55 parts.
The The performance test results that present embodiment prepares binding agent S3 sees Table 1.
Comparative Examples
The preparation method is substantially the same manner as Example 1, and only the methyl alcohol with all uses among the embodiment 1 all replaces with water, finally prepares binding agent C1, and its The performance test results sees Table 1.
Checking example 1
The binding agent for preparing in embodiment 1-6 and the Comparative Examples is carried out the tensile strength test, use furane resin 8 blocks to detect, the resin add-on accounts for roughing sand 1%, and sulfonic acid class solidifying agent add-on is 40% of furane resin.8 blocks are ruptured along the axle center, and binding agent is smeared to fracture place carry out Elongation test and shearing test.Test environment, temperature are 30 ℃, and humidity is R=80%.Test result sees Table 1.
Table 1
By the data in the above-mentioned table 1 as can be seen, binding agent is after placing 2 hours under the condition of hot and humid degree among the present invention, and intensity is apparently higher than the binding agent that adopts the water solvent preparation; Binding agent of the present invention is not obvious with prolonging the back strength retrogression storage period.
Checking example 2
Use furane resin 8 blocks to detect the binding agent A3 of preparation in the embodiment of the invention 3, the resin add-on accounts for roughing sand 1%, sulfonic acid class solidifying agent add-on is 50% of furane resin, 8 blocks is ruptured along the axle center, and binding agent is smeared to fracture place carry out Elongation test and shearing test.Test environment, temperature are 20 ℃, and humidity is R=60%.Test result sees Table 2.
Table 2
| Set time | Tensile strength | Shearing resistance |
| 0.5 hour | 0.67MPa | 1.74MPa |
| 1 hour | 1.25MPa | 3.25MPa |
| 2 hours | 1.75MPa | 4.55MPa |
| 4 hours | 1.63MPa | 1.88MPa |
| 6 hours | 1.64MPa | 4.24MPa |
| 24 hours | 1.65MPa | 4.29MPa |
| 48 hours | 1.58MPa | 4.11MPa |
| 72 hours | 1.50MPa | 3.90MPa |
| 96 hours | 1.41MPa | 3.67MPa |
| 120 hours | 1.38MPa | 3.59MPa |
As can be seen from the above table data, the tensile strength of the binding agent for preparing among the present invention can reach about 1.5MPa in 1-2 hour, and prolongation along with storage period, the tensile strength of binding agent does not obviously reduce, and illustrates to adopt the alcoholic solvent system can overcome the destruction of water solvent system to the binding agent performance greatly.
In sum, the binding agent that the present invention produces has characteristics such as intensity height, anti-hydrolysis, curing speed be fast, can realize substantially solidifying in 30 minutes, and tensile strength all can reach more than the 1.5Mpa in 2 hours.Proof was placed under the natural condition after 120 hours by experiment, and most of adhesive strength of the present invention's preparation still guarantees more than 1.5Mpa, and the cohesive strength strength retrogression is less relatively.The binding agent of the present invention's preparation can be widely used in the bonding of cores such as resin sand, sodium silicate sand, clay-bonded sand, oil-sand and repair.
Obviously, the foregoing description only is for example clearly is described, and is not the qualification to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being extended out thus or change still belong among the protection domain of claim of the present invention.
Claims (10)
1, a kind of binding agent, described binding agent comprises and mainly comprises polyvinyl acetate (PVA) latex and refractory powder, with described binding agent is an integral body, the parts by weight of described polyvinyl acetate (PVA) latex are 35-65 part, the parts by weight of described refractory powder are 40-70 part, and described polyvinyl acetate (PVA) latex draws agent initiated polymerization by chemistry by vinyl acetate and carboxylicesters and forms in alcoholic solvent; Viscosity is the 800-2000 centipoise.
2, binding agent according to claim 1 is characterized in that: as a whole with described polyvinyl acetate (PVA) latex, each raw materials in part by weight that polymerization forms described polyvinyl acetate (PVA) latex is respectively:
Vinyl acetate 20-50 part;
Carboxylicesters 5-25 part;
Alcoholic solvent 10-35 part;
Initiator 0.03-1.3 part.
3, binding agent according to claim 2 is characterized in that: described initiator is ammonium persulphate and/or peroxidation two acyls.
4, binding agent according to claim 3 is characterized in that: described initiator is the mixture of ammonium persulphate and peroxidation two acyls, and both weight ratios are 1:1-2:1.
5, binding agent according to claim 1 and 2 is characterized in that: described carboxylicesters is one or more in acrylate, methacrylic ester, Isooctyl acrylate monomer, butyl acrylate, vinyl acetic monomer, the N-BUTYL ACETATE.
6, binding agent according to claim 1 and 2 is characterized in that: described alcoholic solvent is methyl alcohol and/or ethanol.
7, binding agent according to claim 1 and 2 is characterized in that: described refractory powder is one or more in talcum powder, silica powder, kaolin, clay, the bauxitic clay.
8, the preparation method of the described binding agent of one of claim 1 to 7 comprises the steps:
A) polymerization procedure: earlier initiator is dissolved in the alcoholic solvent and treats to form the initiator alcoholic solution, again with vinyl acetate, carboxylicesters mixes to form mix monomer, the described mix monomer of 50-80% (weight) is added in the reactor, constantly slowly add the described initiator alcoholic solution of part under the condition of stirring for the first time, after polyreaction 0.5-2.5 hour, all join the described mix monomer of remaining 20-50% (weight) in the described reactor slowly again, and in adding the process of described residue mix monomer, slowly repeatedly add remaining described initiator alcoholic solution for the second time, temperature is controlled at 55-75 ℃ in the whole polymerization process, stop polyreaction when mixture viscosity at room temperature is the 500-1000 centipoise in reactor, and obtain polymerisate;
B) dilution step: in described polymerisate, add alcoholic solvent, obtain the polyvinyl acetate (PVA) latex after fully stirring;
C) blending dispersion step: under stirring condition, slowly repeatedly add refractory powder in the described polyvinyl acetate (PVA) latex that in polymerization procedure, obtains, stop when at room temperature viscosity is the 4000-10000 centipoise adding until mixture, and finally obtain described binding agent, wherein, with described binding agent is an integral body, and the parts by weight of described polyvinyl acetate (PVA) latex are 35-65 part, and the parts by weight of described refractory powder are 40-70 part.
9, preparation method according to claim 8 is characterized in that: described initiator is the mixture of ammonium persulphate and peroxidation two acyls, and both weight ratios are 1:1-2:1.
10, preparation method according to claim 8 is characterized in that: described carboxylicesters is one or more in acrylate, methacrylic ester, Isooctyl acrylate monomer, butyl acrylate, vinyl acetic monomer, the N-BUTYL ACETATE; Described alcoholic solvent is methyl alcohol and/or ethanol; Described refractory powder is one or more in talcum powder, silica powder, kaolin, clay, the bauxitic clay.
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| CN103484040A (en) * | 2013-09-22 | 2014-01-01 | 抚顺哥俩好化学有限公司 | Environment-friendly nail-free glue for construction and preparation method thereof |
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| CN101475785B (en) | 2013-04-03 |
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