CN107629751A - A kind of architectural engineering marble glue caking agent and its preparation technology - Google Patents

A kind of architectural engineering marble glue caking agent and its preparation technology Download PDF

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CN107629751A
CN107629751A CN201710912059.1A CN201710912059A CN107629751A CN 107629751 A CN107629751 A CN 107629751A CN 201710912059 A CN201710912059 A CN 201710912059A CN 107629751 A CN107629751 A CN 107629751A
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parts
component
weight
agent
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甘勇
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Fuzhou Cheng Heng Building Materials Co Ltd
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Fuzhou Cheng Heng Building Materials Co Ltd
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Abstract

The invention discloses a kind of architectural engineering marble glue caking agent and its preparation technology, including component A and component B, component A and component B weight ratio are 10:3;Component A is made up of the raw material of following parts by weight:Unsaturated polyester resin, reinforcer, polymerization inhibitor, accelerator, enhanced short fiber, polyethylene glycol methacrylate-styrene polymer, diluent and thixotropic agent;Component B is made up of the raw material of following parts by weight:Filler curing agent, plasticizer, emulsifying agent and thixotropic agent, preparation method of the invention are:Unsaturated-resin is prepared, polyethylene glycol methacrylate-styrene polymer is prepared, prepares component A, prepares component B and prepare marble glue caking agent;The present invention has outstanding tensile-sbear strength and impact strength, has raw material sources convenient, manufacture craft is simple, products obtained therefrom hardening time is moderate, stable storing, and smell is small, and the advantages that hardness is high, good toughness, and adhesive strength is excellent, elasticity is good, color inhibition and wet-hot aging performance are excellent.

Description

A kind of architectural engineering marble glue caking agent and its preparation technology
Technical field
The present invention relates to construction engineering technical field, specially a kind of architectural engineering is with marble glue caking agent and its prepares work Skill.
Background technology
Cloud stone glue is widely used in bonding between all kinds of stone materials or for such as crack of stone surface, hole, sand holes Etc flaw fill up and the repairing to stone material mark of break.Cloud stone glue has point of one pack system and bi-component, due to bi-component marble Glue has the strong points such as gelation rate is fast, hardening time is short and adhesive strength is high relative to one pack system cloud stone glue, thus universal at present Use bi-component cloud stone glue.At present, cloud stone glue is widely used in crack and the mark of break of the bonding or stone surface between all kinds of stone materials Repairing, the performance of cloud stone glue is mainly reflected in hardness, toughness, fixed line speed, polishability etc., but existing cloud stone glue The defects of with intensity difference, air-drying property difference.Influence the construction safety of stone material and the convenience of post processing.
So how to design a kind of architectural engineering marble glue caking agent and its preparation technology, turning into us will currently solve Certainly the problem of.
The content of the invention
The present invention provides a kind of architectural engineering marble glue caking agent and its preparation technology, have outstanding tensile-sbear strength with And impact strength, have raw material sources convenient, manufacture craft is simple, and products obtained therefrom hardening time is moderate, stable storing, smell The advantages that small, and hardness is high, good toughness, and adhesive strength is excellent, elasticity is good, color inhibition and wet-hot aging performance are excellent, can be effective Solve the problems, such as in above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme:A kind of architectural engineering marble glue caking agent, including Component A and component B, the component A and component B weight ratio are 10:3;The component A by following parts by weight raw material group Into:Unsaturated polyester resin 48-52 parts, reinforcer 20-60 parts, polymerization inhibitor 0.05-0.4 parts, accelerator 0.03-0.3 parts, increasing Strong chopped strand 10-20 parts, polyethylene glycol methacrylate-styrene polymer 50-80 parts, diluent 5-20 parts and thixotropic agent 1-3 parts;It is described Component B is made up of the raw material of following parts by weight:Filler curing agent 40-60 parts, plasticizer 35-45 parts, emulsifying agent 0.5-1.5 parts With thixotropic agent 1-3 parts.
A kind of architectural engineering marble glue caking agent preparation technology, comprises the following steps:
1)Prepare unsaturated-resin:Phthalic anhydride, cis-butenedioic anhydride, dihydric alcohol and styrene are weighed by weight percentage, wherein, it will first weigh Phthalic anhydride, cis-butenedioic anhydride and dihydric alcohol put into reactor, be warming up to 105-115 DEG C, start agitator;Then liquid temperature is increased to Reaction takes place at 150-160 DEG C, vapor space still column temperature rises, insulation reaction 20-40 minutes, wherein, column temperature control Below 103 DEG C;And then 190-200 DEG C is progressively warming up to, insulation reaction to acid number is 50-70, starts to vacuumize;Work as acid number 20-25 is down to, stops vacuumizing;Obtained product is finally used into styrene in kettle is diluted under 70-80 DEG C of temperature conditionss It is diluted, that is, obtains unsaturated-resin;
2)Prepare polyethylene glycol methacrylate-styrene polymer:Methacrylic acid, polyethylene glycol 200, polymerization inhibitor, hydrochloric acid are added into reaction Kettle, stirring, is heated to flowing back, and maintains to be reacted at this temperature;Reaction terminates, and cooling, obtains polyethylene glycol metering system Acid esters;
3)Prepare component A:By the unsaturated polyester resin weighed in parts by weight, polyethylene glycol methacrylate-styrene polymer, diluent, Polymerization inhibitor and accelerator are put into the reaction vessel with agitator successively to be stirred, and is then touched what is weighed in parts by weight Become in agent 1-3 parts input reaction vessel, high-speed stirred, then put into reaction vessel the reinforcer weighed in parts by weight and Enhanced short fiber, then stir, vacuumize, blowing, obtain component A;The mixing time wherein to stir is 10-20min, The time of high-speed stirred is 10-15min, and the time then stirred is 15-30min;
4)Prepare component B:The curing agent weighed in parts by weight and plasticizer are sequentially added into the reaction vessel with agitator In stir evenly, the emulsifying agent weighed in parts by weight is then added into reaction vessel and continues to stir, most backward reaction vessel Middle to add the thixotropic agent weighed in parts by weight, scattered stirring, discharging, component B are obtained at a high speed;The time wherein stirred evenly is 10- 15min, the time for continuing to stir are 5-10min, and the time of scattered stirring is 10-15min at a high speed;
5)Prepare marble glue caking agent:Component A and component B is mixed according to above-mentioned weight ratio, produces marble gluing knot Agent.
According to above-mentioned technical proposal, the preparation method of the polymerization inhibitor is:First weigh 40g sodium hydroxides and be put into 500mL burnings In cup, 250mL deionized waters are added into beaker, are stirred, until sodium hydroxide is completely dissolved, then added into beaker 30g SiO 2 powders, stirring stand 15min until after well mixed;Wait after the completion of standing, it is turbid that mixing is added into beaker The mass fraction of liquid quality 10% is 25% hydrochloric acid, and stirring is until have translucent sticky matter to produce, then beaker is placed in into shaking table In, after vibrating 30min, beaker is taken out, and the material adhered on wall of cup is scraped, as sodium metasilicate;By solid-liquid mass ratio 1: 2, the sodium metasilicate of above-mentioned preparation is stirred with deionized water and is well mixed, and it is heated, stir, control while heating Heating-up temperature processed is 70 °C, and the heat time is 45 °C;After the completion of to be heated, it is naturally cooled to room temperature, filter, collect filtering Thing, by solid-liquid mass ratio 2:3, the filtrate of collection is stirred with mass fraction for 30% hydrofluoric acid and mixed, control stirring Speed is 120r/min, after stirring reaction 45min, stands 15min;After standing terminates, the mixture after above-mentioned standing is moved Into the round-bottomed flask of connection reflux condenser, and it is 35% second to add the mass fraction of mixture quality 40% into round-bottomed flask Alcohol, it is stirred until after uniformly, flask is heated, it is 60 °C to control temperature, heats 40min, carries out refluxing extraction 3 It is secondary, merge extract solution;The extract solution of above-mentioned merging is placed in rotary evaporator, rotary evaporation is concentrated into original volume 1/2, then Concentrate is heated, it is 85 °C to control heating-up temperature, and after heating 20min, standing is cooled to room temperature, you can obtains styrene Polymerization inhibitor.
According to above-mentioned technical proposal, the preparation method of the emulsifying agent is:First, that polyamine compounds are dissolved in into alcohols is molten In agent, aldehyde compound is added dropwise under agitation, obtains aldehyde amine intermediate;Then, alkylphenol compoundses are dissolved in alcohols In solvent, aldehyde amine intermediate is added under agitation, is evaporated under reduced pressure after removing 50% solvent, that is, is obtained emulsifying agent.
According to above-mentioned technical proposal, the preparation method of the thixotropic agent is:In mass ratio 2:3, take carclazyte and vermiculite to be put into Milled in grinding mill, cross 50 mesh sieves, collected sieving particle and be put into calcining furnace, design temperature is to calcine, cool to the furnace Room temperature, count in parts by weight, take calcined material, the hydrogen peroxide of mass fraction 15%, lecithin, 3-5 parts tyrosine and dodecyl sulphur Alcohol, it is put into autoclave;Hydrogen shield is used to above-mentioned autoclave, and boosts to 0.6MPa, design temperature, with 130r/min whip modified 5h, standard atmospheric pressure is then depressurized to, then 80 °C are cooled to 4 °C/min, discharged, will discharge while hot Thing is placed in liquid nitrogen quick cooler, freezing processing, collects frozen material, and warms naturally to room temperature, is filtered, and collects filter residue, standby With;Take biogas slurry to be filtered under diminished pressure, collect filtrate, count in parts by weight, take filtrate, peptone, yeast extract, soybean oil and 1- 4 parts of egg yolks, are put into fermentation tank, and design temperature is 37 °C, sealed fermenter, then right with 100r/min stirrings fermentation 3 days Fermenting mixture in fermentation tank is filtered under diminished pressure, and collects filtrate;In mass ratio 1:4-1:2, by standby filter residue and above-mentioned filter Liquid is put into container, and container is placed in ultrasonator, sonic oscillation, then is stood overnight, and is filtered then to being added in container The sodium hydride of slag amount 0.8%, the air in container is discharged using monosilane, container is heated, 5h is stirred with 200r/min Afterwards, room temperature is naturally cooled to, mixture in container is put into the 70% of original volume is concentrated into vacuum concentration pot, collects concentration Thing, you can obtain thixotropic agent.
According to above-mentioned technical proposal, the step 2)The percentage by weight of unsaturated-resin each component is:Phthalic anhydride 23-27%, Cis-butenedioic anhydride 15-20%, 25-35% and styrene 25-35%.
According to above-mentioned technical proposal, the step 2)With step 3)Temperature during middle stirring is 30-40 DEG C.
Compared with prior art, beneficial effects of the present invention:With outstanding tensile-sbear strength and impact strength, have Raw material sources are convenient, and manufacture craft is simple, and products obtained therefrom hardening time is moderate, and stable storing, smell is small, and hardness is high, toughness Well, the advantages that adhesive strength is excellent, elasticity is good, color inhibition and wet-hot aging performance are excellent.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and a part for constitution instruction, the reality with the present invention Apply example to be used to explain the present invention together, be not construed as limiting the invention.
In the accompanying drawings:
Fig. 1 is the preparation flow figure of the present invention.
Embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that described herein preferred real Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1:As shown in figure 1, the present invention provides a kind of architectural engineering marble glue caking agent, including component A and group The weight ratio for dividing B, the component A and component B is 10:3;The component A is made up of the raw material of following parts by weight:Unsaturation is poly- 48 parts of ester resin, 20 parts of reinforcer, 0.05 part of polymerization inhibitor, 0.03 part of accelerator, 10 parts of enhanced short fiber, polyethylene glycol first 1 part of 50 parts of base acrylate, diluent 5 and thixotropic agent;The component B is made up of the raw material of following parts by weight:Filler solidifies 1 part of agent 40-60 parts, plasticizer 35-45 parts, 0.5 part of emulsifying agent and thixotropic agent.
A kind of architectural engineering marble glue caking agent preparation technology, comprises the following steps:
1)Prepare unsaturated-resin:Phthalic anhydride, cis-butenedioic anhydride, dihydric alcohol and styrene are weighed by weight percentage, wherein, it will first weigh Phthalic anhydride, cis-butenedioic anhydride and dihydric alcohol put into reactor, be warming up to 105-115 DEG C, start agitator;Then liquid temperature is increased to Reaction takes place at 150-160 DEG C, vapor space still column temperature rises, insulation reaction 20-40 minutes, wherein, column temperature control Below 103 DEG C;And then 190-200 DEG C is progressively warming up to, insulation reaction to acid number is 50-70, starts to vacuumize;Work as acid number 20-25 is down to, stops vacuumizing;Obtained product is finally used into styrene in kettle is diluted under 70-80 DEG C of temperature conditionss It is diluted, that is, obtains unsaturated-resin;
2)Prepare polyethylene glycol methacrylate-styrene polymer:Methacrylic acid, polyethylene glycol 200, polymerization inhibitor, hydrochloric acid are added into reaction Kettle, stirring, is heated to flowing back, and maintains to be reacted at this temperature;Reaction terminates, and cooling, obtains polyethylene glycol metering system Acid esters;
3)Prepare component A:By the unsaturated polyester resin weighed in parts by weight, polyethylene glycol methacrylate-styrene polymer, diluent, Polymerization inhibitor and accelerator are put into the reaction vessel with agitator successively to be stirred, and is then touched what is weighed in parts by weight Become in agent 1-3 parts input reaction vessel, high-speed stirred, then put into reaction vessel the reinforcer weighed in parts by weight and Enhanced short fiber, then stir, vacuumize, blowing, obtain component A;The mixing time wherein to stir is 10-20min, The time of high-speed stirred is 10-15min, and the time then stirred is 15-30min;
4)Prepare component B:The curing agent weighed in parts by weight and plasticizer are sequentially added into the reaction vessel with agitator In stir evenly, the emulsifying agent weighed in parts by weight is then added into reaction vessel and continues to stir, most backward reaction vessel Middle to add the thixotropic agent weighed in parts by weight, scattered stirring, discharging, component B are obtained at a high speed;The time wherein stirred evenly is 10- 15min, the time for continuing to stir are 5-10min, and the time of scattered stirring is 10-15min at a high speed;
5)Prepare marble glue caking agent:Component A and component B is mixed according to above-mentioned weight ratio, produces marble gluing knot Agent.
According to above-mentioned technical proposal, the preparation method of the polymerization inhibitor is:First weigh 40g sodium hydroxides and be put into 500mL burnings In cup, 250mL deionized waters are added into beaker, are stirred, until sodium hydroxide is completely dissolved, then added into beaker 30g SiO 2 powders, stirring stand 15min until after well mixed;Wait after the completion of standing, it is turbid that mixing is added into beaker The mass fraction of liquid quality 10% is 25% hydrochloric acid, and stirring is until have translucent sticky matter to produce, then beaker is placed in into shaking table In, after vibrating 30min, beaker is taken out, and the material adhered on wall of cup is scraped, as sodium metasilicate;By solid-liquid mass ratio 1: 2, the sodium metasilicate of above-mentioned preparation is stirred with deionized water and is well mixed, and it is heated, stir, control while heating Heating-up temperature processed is 70 °C, and the heat time is 45 °C;After the completion of to be heated, it is naturally cooled to room temperature, filter, collect filtering Thing, by solid-liquid mass ratio 2:3, the filtrate of collection is stirred with mass fraction for 30% hydrofluoric acid and mixed, control stirring Speed is 120r/min, after stirring reaction 45min, stands 15min;After standing terminates, the mixture after above-mentioned standing is moved Into the round-bottomed flask of connection reflux condenser, and it is 35% second to add the mass fraction of mixture quality 40% into round-bottomed flask Alcohol, it is stirred until after uniformly, flask is heated, it is 60 °C to control temperature, heats 40min, carries out refluxing extraction 3 It is secondary, merge extract solution;The extract solution of above-mentioned merging is placed in rotary evaporator, rotary evaporation is concentrated into original volume 1/2, then Concentrate is heated, it is 85 °C to control heating-up temperature, and after heating 20min, standing is cooled to room temperature, you can obtains styrene Polymerization inhibitor.
According to above-mentioned technical proposal, the preparation method of the emulsifying agent is:First, that polyamine compounds are dissolved in into alcohols is molten In agent, aldehyde compound is added dropwise under agitation, obtains aldehyde amine intermediate;Then, alkylphenol compoundses are dissolved in alcohols In solvent, aldehyde amine intermediate is added under agitation, is evaporated under reduced pressure after removing 50% solvent, that is, is obtained emulsifying agent.
According to above-mentioned technical proposal, the preparation method of the thixotropic agent is:In mass ratio 2:3, take carclazyte and vermiculite to be put into Milled in grinding mill, cross 50 mesh sieves, collected sieving particle and be put into calcining furnace, design temperature is to calcine, cool to the furnace Room temperature, count in parts by weight, take calcined material, the hydrogen peroxide of mass fraction 15%, lecithin, 3-5 parts tyrosine and dodecyl sulphur Alcohol, it is put into autoclave;Hydrogen shield is used to above-mentioned autoclave, and boosts to 0.6MPa, design temperature, with 130r/min whip modified 5h, standard atmospheric pressure is then depressurized to, then 80 °C are cooled to 4 °C/min, discharged, will discharge while hot Thing is placed in liquid nitrogen quick cooler, freezing processing, collects frozen material, and warms naturally to room temperature, is filtered, and collects filter residue, standby With;Take biogas slurry to be filtered under diminished pressure, collect filtrate, count in parts by weight, take filtrate, peptone, yeast extract, soybean oil and 1- 4 parts of egg yolks, are put into fermentation tank, and design temperature is 37 °C, sealed fermenter, then right with 100r/min stirrings fermentation 3 days Fermenting mixture in fermentation tank is filtered under diminished pressure, and collects filtrate;In mass ratio 1:4-1:2, by standby filter residue and above-mentioned filter Liquid is put into container, and container is placed in ultrasonator, sonic oscillation, then is stood overnight, and is filtered then to being added in container The sodium hydride of slag amount 0.8%, the air in container is discharged using monosilane, container is heated, 5h is stirred with 200r/min Afterwards, room temperature is naturally cooled to, mixture in container is put into the 70% of original volume is concentrated into vacuum concentration pot, collects concentration Thing, you can obtain thixotropic agent.
According to above-mentioned technical proposal, the step 2)The percentage by weight of unsaturated-resin each component is:Phthalic anhydride 23-27%, Cis-butenedioic anhydride 15-20%, 25-35% and styrene 25-35%.
According to above-mentioned technical proposal, the step 2)With step 3)Temperature during middle stirring is 30-40 DEG C.
Embodiment 2:As shown in figure 1, the present invention provides a kind of architectural engineering marble glue caking agent, including component A and group The weight ratio for dividing B, the component A and component B is 10:3;The component A is made up of the raw material of following parts by weight:Unsaturation is poly- 52 parts of ester resin, 60 parts of reinforcer, 0.4 part of polymerization inhibitor, 0.3 part of accelerator, 20 parts of enhanced short fiber, polyethylene glycol methyl 3 parts of 80 parts of acrylate, diluent 20 and thixotropic agent;The component B is made up of the raw material of following parts by weight:Filler curing agent 3 parts of 60 parts, 45 parts of plasticizer, 1.5 parts of emulsifying agent and thixotropic agent.
A kind of architectural engineering marble glue caking agent preparation technology, comprises the following steps:
1)Prepare unsaturated-resin:Phthalic anhydride, cis-butenedioic anhydride, dihydric alcohol and styrene are weighed by weight percentage, wherein, it will first weigh Phthalic anhydride, cis-butenedioic anhydride and dihydric alcohol put into reactor, be warming up to 105-115 DEG C, start agitator;Then liquid temperature is increased to Reaction takes place at 150-160 DEG C, vapor space still column temperature rises, insulation reaction 20-40 minutes, wherein, column temperature control Below 103 DEG C;And then 190-200 DEG C is progressively warming up to, insulation reaction to acid number is 50-70, starts to vacuumize;Work as acid number 20-25 is down to, stops vacuumizing;Obtained product is finally used into styrene in kettle is diluted under 70-80 DEG C of temperature conditionss It is diluted, that is, obtains unsaturated-resin;
2)Prepare polyethylene glycol methacrylate-styrene polymer:Methacrylic acid, polyethylene glycol 200, polymerization inhibitor, hydrochloric acid are added into reaction Kettle, stirring, is heated to flowing back, and maintains to be reacted at this temperature;Reaction terminates, and cooling, obtains polyethylene glycol metering system Acid esters;
3)Prepare component A:By the unsaturated polyester resin weighed in parts by weight, polyethylene glycol methacrylate-styrene polymer, diluent, Polymerization inhibitor and accelerator are put into the reaction vessel with agitator successively to be stirred, and is then touched what is weighed in parts by weight Become in agent 1-3 parts input reaction vessel, high-speed stirred, then put into reaction vessel the reinforcer weighed in parts by weight and Enhanced short fiber, then stir, vacuumize, blowing, obtain component A;The mixing time wherein to stir is 10-20min, The time of high-speed stirred is 10-15min, and the time then stirred is 15-30min;
4)Prepare component B:The curing agent weighed in parts by weight and plasticizer are sequentially added into the reaction vessel with agitator In stir evenly, the emulsifying agent weighed in parts by weight is then added into reaction vessel and continues to stir, most backward reaction vessel Middle to add the thixotropic agent weighed in parts by weight, scattered stirring, discharging, component B are obtained at a high speed;The time wherein stirred evenly is 10- 15min, the time for continuing to stir are 5-10min, and the time of scattered stirring is 10-15min at a high speed;
5)Prepare marble glue caking agent:Component A and component B is mixed according to above-mentioned weight ratio, produces marble gluing knot Agent.
According to above-mentioned technical proposal, the preparation method of the polymerization inhibitor is:First weigh 40g sodium hydroxides and be put into 500mL burnings In cup, 250mL deionized waters are added into beaker, are stirred, until sodium hydroxide is completely dissolved, then added into beaker 30g SiO 2 powders, stirring stand 15min until after well mixed;Wait after the completion of standing, it is turbid that mixing is added into beaker The mass fraction of liquid quality 10% is 25% hydrochloric acid, and stirring is until have translucent sticky matter to produce, then beaker is placed in into shaking table In, after vibrating 30min, beaker is taken out, and the material adhered on wall of cup is scraped, as sodium metasilicate;By solid-liquid mass ratio 1: 2, the sodium metasilicate of above-mentioned preparation is stirred with deionized water and is well mixed, and it is heated, stir, control while heating Heating-up temperature processed is 70 °C, and the heat time is 45 °C;After the completion of to be heated, it is naturally cooled to room temperature, filter, collect filtering Thing, by solid-liquid mass ratio 2:3, the filtrate of collection is stirred with mass fraction for 30% hydrofluoric acid and mixed, control stirring Speed is 120r/min, after stirring reaction 45min, stands 15min;After standing terminates, the mixture after above-mentioned standing is moved Into the round-bottomed flask of connection reflux condenser, and it is 35% second to add the mass fraction of mixture quality 40% into round-bottomed flask Alcohol, it is stirred until after uniformly, flask is heated, it is 60 °C to control temperature, heats 40min, carries out refluxing extraction 3 It is secondary, merge extract solution;The extract solution of above-mentioned merging is placed in rotary evaporator, rotary evaporation is concentrated into original volume 1/2, then Concentrate is heated, it is 85 °C to control heating-up temperature, and after heating 20min, standing is cooled to room temperature, you can obtains styrene Polymerization inhibitor.
According to above-mentioned technical proposal, the preparation method of the emulsifying agent is:First, that polyamine compounds are dissolved in into alcohols is molten In agent, aldehyde compound is added dropwise under agitation, obtains aldehyde amine intermediate;Then, alkylphenol compoundses are dissolved in alcohols In solvent, aldehyde amine intermediate is added under agitation, is evaporated under reduced pressure after removing 50% solvent, that is, is obtained emulsifying agent.
According to above-mentioned technical proposal, the preparation method of the thixotropic agent is:In mass ratio 2:3, take carclazyte and vermiculite to be put into Milled in grinding mill, cross 50 mesh sieves, collected sieving particle and be put into calcining furnace, design temperature is to calcine, cool to the furnace Room temperature, count in parts by weight, take calcined material, the hydrogen peroxide of mass fraction 15%, lecithin, 3-5 parts tyrosine and dodecyl sulphur Alcohol, it is put into autoclave;Hydrogen shield is used to above-mentioned autoclave, and boosts to 0.6MPa, design temperature, with 130r/min whip modified 5h, standard atmospheric pressure is then depressurized to, then 80 °C are cooled to 4 °C/min, discharged, will discharge while hot Thing is placed in liquid nitrogen quick cooler, freezing processing, collects frozen material, and warms naturally to room temperature, is filtered, and collects filter residue, standby With;Take biogas slurry to be filtered under diminished pressure, collect filtrate, count in parts by weight, take filtrate, peptone, yeast extract, soybean oil and 1- 4 parts of egg yolks, are put into fermentation tank, and design temperature is 37 °C, sealed fermenter, then right with 100r/min stirrings fermentation 3 days Fermenting mixture in fermentation tank is filtered under diminished pressure, and collects filtrate;In mass ratio 1:4-1:2, by standby filter residue and above-mentioned filter Liquid is put into container, and container is placed in ultrasonator, sonic oscillation, then is stood overnight, and is filtered then to being added in container The sodium hydride of slag amount 0.8%, the air in container is discharged using monosilane, container is heated, 5h is stirred with 200r/min Afterwards, room temperature is naturally cooled to, mixture in container is put into the 70% of original volume is concentrated into vacuum concentration pot, collects concentration Thing, you can obtain thixotropic agent.
According to above-mentioned technical proposal, the step 2)The percentage by weight of unsaturated-resin each component is:Phthalic anhydride 23-27%, Cis-butenedioic anhydride 15-20%, 25-35% and styrene 25-35%.
According to above-mentioned technical proposal, the step 2)With step 3)Temperature during middle stirring is 30-40 DEG C.
Based on above-mentioned, it is an advantage of the current invention that with outstanding tensile-sbear strength and impact strength, there is raw material Source is convenient, and manufacture craft is simple, and products obtained therefrom hardening time is moderate, and stable storing, smell is small, and hardness is high, good toughness, bonding The advantages that good strength, good, color inhibition and wet-hot aging performance are excellent elasticity.
Finally it should be noted that:The preferred embodiment of the present invention is the foregoing is only, is not intended to limit the invention, to the greatest extent The present invention is described in detail with reference to the foregoing embodiments for pipe, and for those skilled in the art, it still can be with Technical scheme described in foregoing embodiments is modified, or equivalent substitution is carried out to which part technical characteristic.It is all Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., it should be included in the guarantor of the present invention Within the scope of shield.

Claims (7)

1. a kind of architectural engineering marble glue caking agent, including component A and component B, it is characterised in that:The component A and component B Weight ratio be 10:3;The component A is made up of the raw material of following parts by weight:Unsaturated polyester resin 48-52 parts, enhancing are filled out Expect 20-60 parts, polymerization inhibitor 0.05-0.4 parts, accelerator 0.03-0.3 parts, enhanced short fiber 10-20 parts, polyethylene glycol methyl Acrylate 50-80 parts, diluent 5-20 parts and thixotropic agent 1-3 parts;The component B is made up of the raw material of following parts by weight: Filler curing agent 40-60 parts, plasticizer 35-45 parts, emulsifying agent 0.5-1.5 parts and thixotropic agent 1-3 parts.
A kind of 2. architectural engineering marble glue caking agent preparation technology, it is characterised in that:Comprise the following steps:
1)Prepare unsaturated-resin:Phthalic anhydride, cis-butenedioic anhydride, dihydric alcohol and styrene are weighed by weight percentage, wherein, it will first weigh Phthalic anhydride, cis-butenedioic anhydride and dihydric alcohol put into reactor, be warming up to 105-115 DEG C, start agitator;Then liquid temperature is increased to Reaction takes place at 150-160 DEG C, vapor space still column temperature rises, insulation reaction 20-40 minutes, wherein, column temperature control Below 103 DEG C;And then 190-200 DEG C is progressively warming up to, insulation reaction to acid number is 50-70, starts to vacuumize;Work as acid number 20-25 is down to, stops vacuumizing;Obtained product is finally used into styrene in kettle is diluted under 70-80 DEG C of temperature conditionss It is diluted, that is, obtains unsaturated-resin;
2)Prepare polyethylene glycol methacrylate-styrene polymer:Methacrylic acid, polyethylene glycol 200, polymerization inhibitor, hydrochloric acid are added into reaction Kettle, stirring, is heated to flowing back, and maintains to be reacted at this temperature;Reaction terminates, and cooling, obtains polyethylene glycol metering system Acid esters;
3)Prepare component A:By the unsaturated polyester resin weighed in parts by weight, polyethylene glycol methacrylate-styrene polymer, diluent, Polymerization inhibitor and accelerator are put into the reaction vessel with agitator successively to be stirred, and is then touched what is weighed in parts by weight Become in agent 1-3 parts input reaction vessel, high-speed stirred, then put into reaction vessel the reinforcer weighed in parts by weight and Enhanced short fiber, then stir, vacuumize, blowing, obtain component A;The mixing time wherein to stir is 10-20min, The time of high-speed stirred is 10-15min, and the time then stirred is 15-30min;
4)Prepare component B:The curing agent weighed in parts by weight and plasticizer are sequentially added into the reaction vessel with agitator In stir evenly, the emulsifying agent weighed in parts by weight is then added into reaction vessel and continues to stir, most backward reaction vessel Middle to add the thixotropic agent weighed in parts by weight, scattered stirring, discharging, component B are obtained at a high speed;The time wherein stirred evenly is 10- 15min, the time for continuing to stir are 5-10min, and the time of scattered stirring is 10-15min at a high speed;
5)Prepare marble glue caking agent:Component A and component B is mixed according to above-mentioned weight ratio, produces marble gluing knot Agent.
A kind of 3. architectural engineering marble glue caking agent according to claim 1, it is characterised in that:The system of the polymerization inhibitor Preparation Method is:First weigh 40g sodium hydroxides to be put into 500mL beakers, 250mL deionized waters added into beaker, are stirred, Until sodium hydroxide is completely dissolved, then adds 30g SiO 2 powders into beaker, stirring is stood until after well mixed 15min;Wait after the completion of standing, it is 25% hydrochloric acid that the mass fraction of mixing turbid quality 10% is added into beaker, and stirring is until have Translucent sticky matter is produced, then beaker is placed in shaking table, and after vibrating 30min, beaker is taken out, and will be adhered on wall of cup Material scrape, as sodium metasilicate;By solid-liquid mass ratio 1:2, the sodium metasilicate of above-mentioned preparation is stirred with deionized water mixed Close uniformly, and it is heated, stirred while heating, it is 70 °C to control heating-up temperature, and the heat time is 45 °C;It is to be heated complete Cheng Hou, it is naturally cooled to room temperature, filter, filtrate is collected, by solid-liquid mass ratio 2:3, by the filtrate and quality of collection Fraction is that 30% hydrofluoric acid is stirred mixing, and it is 120r/min to control mixing speed, after stirring reaction 45min, standing 15min;After standing terminates, the mixture after above-mentioned standing is moved in the round-bottomed flask of connection reflux condenser, and to circle It is 35% ethanol that the mass fraction of mixture quality 40% is added in the flask of bottom, is stirred until after uniformly, flask is added Heat, it is 60 °C to control temperature, heats 40min, carries out refluxing extraction 3 times, merges extract solution;The extract solution of above-mentioned merging is placed in In rotary evaporator, rotary evaporation is concentrated into original volume 1/2, then concentrate is heated, and it is 85 °C to control heating-up temperature, After heating 20min, standing is cooled to room temperature, you can obtains styrene polymerization inhibitor.
A kind of 4. architectural engineering marble glue caking agent according to claim 1, it is characterised in that:The system of the emulsifying agent Preparation Method is:First, polyamine compounds are dissolved in alcohols solvent, aldehyde compound is added dropwise under agitation, obtain aldehyde Amine intermediate;Then, alkylphenol compoundses are dissolved in alcohols solvent, add aldehyde amine intermediate, decompression under agitation After 50% solvent is distilled off, that is, obtain emulsifying agent.
A kind of 5. architectural engineering marble glue caking agent according to claim 1, it is characterised in that:The system of the thixotropic agent Preparation Method is:In mass ratio 2:3, take carclazyte and vermiculite to be put into grinding mill and milled, cross 50 mesh sieves, collect sieving particle and put Enter in calcining furnace, design temperature is to calcine, cool to room temperature with the furnace, count in parts by weight, take calcined material, mass fraction 15% Hydrogen peroxide, lecithin, 3-5 parts tyrosine and lauryl mercaptan, are put into autoclave;Hydrogen is used to above-mentioned autoclave Gas shielded, and boost to 0.6MPa, design temperature, with 130r/min whip modified 5h, then it is depressurized to standard atmospheric pressure, then with 4 °C/min is cooled to 80 °C, discharges while hot, will go out material and is placed in liquid nitrogen quick cooler, freezing processing, collects frozen material, and certainly Room temperature so is warming up to, is filtered, collects filter residue, it is standby;Take biogas slurry to be filtered under diminished pressure, collect filtrate, count in parts by weight, Filtrate, peptone, yeast extract, soybean oil and 1-4 part egg yolks are taken, is put into fermentation tank, design temperature is 37 °C, sealing hair Fermentation tank, with 100r/min stirrings fermentation 3 days, then the fermenting mixture in fermentation tank is filtered under diminished pressure, collects filtrate;Press Mass ratio 1:4-1:2, standby filter residue and above-mentioned filtrate are put into container, and container is placed in ultrasonator, ultrasound is shaken Swing, then stand overnight, then to the sodium hydride that filter residue quality 0.8% is added in container, using monosilane by the air in container Discharge, container is heated, after stirring 5h with 200r/min, naturally cool to room temperature, mixture in container is put into vacuum concentration The 70% of original volume is concentrated into tank, collects concentrate, you can obtains thixotropic agent.
A kind of 6. architectural engineering according to claim 2 marble glue caking agent preparation technology, it is characterised in that:The step Rapid 2)The percentage by weight of unsaturated-resin each component is:Phthalic anhydride 23-27%, cis-butenedioic anhydride 15-20%, 25-35% and styrene 25- 35%。
A kind of 7. architectural engineering according to claim 2 marble glue caking agent preparation technology, it is characterised in that:The step Rapid 3)With step 4)Temperature during middle stirring is 30-40 DEG C.
CN201710912059.1A 2017-09-29 2017-09-29 A kind of architectural engineering marble glue caking agent and its preparation technology Withdrawn CN107629751A (en)

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CN117089309B (en) * 2023-08-28 2024-04-23 江苏大力士投资有限公司 Functional marble adhesive and preparation method thereof

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