CN109825111A - A kind of free from vacuum dehydrating can be used to the pearl filler of production silane modified polyether seal glue - Google Patents

A kind of free from vacuum dehydrating can be used to the pearl filler of production silane modified polyether seal glue Download PDF

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Publication number
CN109825111A
CN109825111A CN201910247240.4A CN201910247240A CN109825111A CN 109825111 A CN109825111 A CN 109825111A CN 201910247240 A CN201910247240 A CN 201910247240A CN 109825111 A CN109825111 A CN 109825111A
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China
Prior art keywords
seal glue
free
modified polyether
silane modified
polyether seal
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CN201910247240.4A
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Chinese (zh)
Inventor
何丽秋
莫淑一
龙飞
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Guilin University of Technology
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Guilin University of Technology
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Abstract

The present invention provides the pearl filler that a kind of free from vacuum dehydrating can be used to production silane modified polyether seal glue, it is related to nonmetallic mineral technical field, the pearl filler obtains by the following method: according to weight ratio calcite in powder: water: by three, ball milling filters grinding aid=1:0.3-1.5:0.001-0.1 after mixing, the activator for accounting for dry powder total weight 0.5-3% is added, in 40-80 DEG C of sufficiently reaction, it is cooling, dehydration to water content is not more than 1%, again through with the dry powder to water content no more than 0.1% of dry machine;The present invention uses wet processing and modification, in conjunction with the mode that two-stage is dry, obtains the calcium carbonate superfine powder powder that water content is lower than 0.1%, meets without agitating and heating vacuum dehydration, and room temperature directly produces the technique requirement of polyether seal glue.

Description

A kind of free from vacuum dehydrating can be used to the carbonic acid of production silane modified polyether seal glue Calcium filler
[technical field]
The present invention relates to nonmetallic mineral technical fields, and in particular to a kind of free from vacuum dehydrating can be used to production silane The pearl filler of modified polyether seal glue.
[background technique]
With the rise of assembled architecture, sealant as a kind of tool that is important, having both sealing and attachment function, R&D and production is concerned.Silane modified polyether seal glue has excellent mechanical strength, figure ornament, resistance to soiling, and without free Isocyanates and organic matter are the main direction of development of domestic and international novel elastic sealant at present.Silane modified polyether seal glue Production process needs to exist to end-silicane-group modified polyether polymer, filler, plasticizer, thixotropic agent, light stabilizer and antioxidant etc. The stirring that 1-2h is carried out at 90-110 DEG C needs in whipping process with vacuumizing, and cooled to room temperature is again after stirring Deicer, coupling agent and catalyst is added and carries out 50 DEG C or less vacuum stirring 0.5h, not only energy consumption is high and production effect for this method Rate is extremely low.
Therefore, inventor is directed to the problem of current silane modified polyether seal glue production process, provides a kind of nothing Palpus vacuum dehydration can be used to the pearl filler of production silane modified polyether seal glue.
[summary of the invention]
In view of this, the purpose of the present invention is to provide a kind of free from vacuum dehydrating can be used to production silane modified polyether The pearl filler of sealant is obtained water content and is lower than using wet processing and modification in conjunction with the mode that two-stage is dry 0.1% calcium carbonate superfine powder powder meets without agitating and heating vacuum dehydration, and the technique that room temperature directly produces polyether seal glue is wanted It asks.
In order to solve the above-mentioned technical problem, present invention employs the following technical solutions:
A kind of free from vacuum dehydrating can be used to the pearl filler of production silane modified polyether seal glue, described without true The pearl filler that sky dehydration can be used to production silane modified polyether seal glue obtains by the following method:
(1) calcite raw material powder, water and grinding aid are mixed according to the ratio that weight ratio is 1:0.3-1.5:0.001-0.1 Uniformly, adding diameter is the mill ball that 0.7-3.0mm accounts for three's weight 30-55%, and being ground to calcium carbonate granule partial size is It 0.5-4 μm, crosses 80-325 mesh and obtains calcium carbonate slurry;
(2) activator for accounting for dry powder total weight 0.5-4% is added in calcium carbonate slurry, it is cold in 40-80 DEG C of sufficiently reaction But, it then is dehydrated to water content no more than 1%, obtains just dry powder body;
(3) the first dry powder body of step (2) is not more than 0.1% through being dried to water content with dry machine, cooling, using 2 layers of paper Add 1 tunic packaging bag packaging can be obtained free from vacuum dehydrating can be used to production silane modified polyether seal glue calcium carbonate fill out Material.
In the present invention, further, the mill ball in the step (1) is alumina ball, zirconium aluminium ceramic ball, oxygen Change one of zirconium ball or Zirconium silicate ceramic ball.
In the present invention, further, in the step (2), it is dehydrated as follows no more than 1% concrete mode to water content: Mistake 80-325 mesh is obtained into calcium carbonate slurry dehydration and is concentrated into water content no more than 25%, then with the speed of 400-1800kg/h Being passed through flow velocity is 5-60m3It is atomized in/s, the air-flow that temperature is 300-450 DEG C, flash distillation to water content is not more than 1%.
In the present invention, further, in the step (1) grinding aid be polyvinyl alcohol, Sodium Polyacrylate, polyphosphate sodium, One of sodium lignin sulfonate and silane coupling agent or their any combination.
In the present invention, further, the activator in the step (2) is in C12~C22 fatty acid and C18 olefin(e) acid The saponification liquor of one or more kinds of arbitrary proportion mixing.
In the present invention, further, it is 15-40 μm that the calcite in powder of the selection in the step (1), which is particle diameter, Calcite in powder.
In the present invention, further, the grinding in the step (1) is by the way of stirring, mixing time 1-5h, stirring Speed is 500-6000r/min.
The additive amount of pearl filler of the present invention is 55-65%, prepares silane modified polyether seal glue by cold process, is used Cold process production is reduction silane modified polyether seal glue production energy consumption and raising production efficiency compared to the advantages of conventional method, Obtained sealant properties are met the requirements.Wherein, a kind of free from vacuum dehydrating of the present invention can be used to production silane The pearl filler index of modified polyether seal glue is as follows: partial size: D50=0.5-1.5 μm, D97≤ 7 μm, calcium carbonate content >= 96%, whiteness >=90;Activation rate >=95%, oil factor 20-50g/100g.
Note: partial size D in product index50It indicates to press quantity statistics average grain diameter, D97It is expressed as the partial size model of 97% powder It encloses;Oil factor indicates the minimum quality of dibutyl phthalate required for making 100g powder agglomerating.
In conclusion by adopting the above-described technical solution, the present invention is include at least the following beneficial effects:
1. the problem that the present invention is high for modified sealant production energy consumption and production efficiency is extremely low improves, by adopting It reacted with wet-process modified, powder surface with activator, be lower than 0.1% using two-step method dehydration and drying, control product moisture content Etc. modes prepare pearl filler, can overcome the problems, such as above-mentioned, the Carbonate Particle Size being prepared is thin, and size distribution It is narrow, calcium carbonate powder is modified by the way of wet-process modified, uniformity is good, and modified effect is good, stores in air and contains for 24 hours Water rate is without significant change;Silane modified polyether seal glue is prepared using pearl filler produced by the present invention, free from vacuum dehydrating, Room temperature in vacuo is stirred, and the properties of product that the present invention obtains are good, can preferably be applied to prepare silane-modified poly- In ether sealant and its Related product.
2. the partial size of the invention in order to reduce calcium carbonate powder, is ground using water mill method, is added in process of lapping Grinding efficiency can be improved in grinding aid, and grinding aid can be attached to powder surface again, reunion degree when reducing dry, to reach To good dispersion effect.
3. the activator that the present invention uses is with the functional group and water-wet side that can be chemically reacted with powder surface The organic matter of base either fatty acid salt, these activators can be dissolved in water, and presence can be with the group generationization of powder surface again The functional group for learning reaction forms chemical bond with the group of powder surface, organic matter is anchored at powder surface, to improve powder Compatibility between polymer is conducive to the intensity for dispersing and improving sealant when preparing silane modified polyether seal glue.
[Detailed description of the invention]
Fig. 1 is the SEM figure of pearl filler product described in the embodiment of the present invention 2.
Attached drawing analysis: with reference to the accompanying drawings it is found that 2 the method according to embodiments of the present invention preparation calcium carbonate filler particles without Corner angle, particle diameter distribution hard aggregation-free between 0.5-4.0 μm, particle, dispersion effect is good, meets de- without agitating and heating vacuum Water, room temperature directly produce the technique requirement of polyether seal glue.
[specific embodiment]
The following examples can help those skilled in the art that the present invention is more fully understood, but cannot be with any Mode limits the present invention.
Embodiment 1
The calcium carbonate that can be used to production silane modified polyether seal glue the present embodiment provides a kind of free from vacuum dehydrating is filled out Material, obtains by the following method:
(1) it is 15 μm of calcite in powder, water and polyvinyl alcohol by diameter to mix according to the ratio that weight ratio is 1:0.3:0.001 Uniformly, adding diameter is the mill ball that 0.7mm accounts for three's weight 30%, each size and additional amount in mill ball are as follows: Zirconium silicate ceramic ball 25%, 1.4-2.0mm Zirconium silicate ceramic ball 15%, the 2.0-2.5mm Zirconium silicate ceramic ball of 0.7-1.4mm 10%, being ground to calcium carbonate granule partial size is 0.5-4.0 μm, crosses 80 meshes and obtains calcium carbonate slurry;Grinding is using the side stirred Formula, mixing time 1h, mixing speed 500r/min;
(2) activator for accounting for dry powder total weight 0.5% is added in calcium carbonate slurry, it is cooling in 40 DEG C of sufficiently reactions, then Dehydration to water content is not more than 1%, obtains just dry powder body;Wherein, it is dehydrated as follows no more than 1% concrete mode to water content: Calcium carbonate slurry dehydration is obtained by filtration in 80 mesh and is concentrated into water content no more than 25%, then flow velocity is passed through with the speed of 400kg/h For 5m3It is atomized in/s, the air-flow that temperature is 300 DEG C, flash distillation to water content is not more than 1%;Activator be in mass ratio be that 1:1 is mixed The stearic acid of conjunction and lauric saponification liquor;
(3) the first dry powder body of step (2) is not more than 0.1% through being dried to water content with dry machine, cooling, using 2 layers of paper Add 1 tunic packaging bag packaging can be obtained free from vacuum dehydrating can be used to production silane modified polyether seal glue calcium carbonate fill out Material.
Embodiment 2
The calcium carbonate that can be used to production silane modified polyether seal glue the present embodiment provides a kind of free from vacuum dehydrating is filled out Material, obtains by the following method:
(1) it is 38 μm of calcite in powder, water and polyphosphate sodium by diameter to mix according to the ratio that weight ratio is 1:0.9:0.08 Uniformly, adding diameter is the mill ball that 0.7-3.0mm accounts for three's weight 55%, and each size additional amount is 0.7- in mill ball Zirconium aluminium ceramic ball 25%, 1.4-2.0mm zirconium aluminium ceramic ball 15%, the 2.0-2.5mm zirconium aluminium ceramic ball of 1.4mm 10%, 2.5-3.0mm zirconium aluminium ceramic ball 5%, being ground to calcium carbonate granule partial size is 0.5-4.0 μm, crosses 200 meshes and obtains Calcium carbonate slurry;Grinding is by the way of stirring, mixing time 3h, mixing speed 1500r/min;
(2) activator for accounting for dry powder total weight 2.5% is added in calcium carbonate slurry, it is cooling in 70 DEG C of sufficiently reactions, then Dehydration to water content is not more than 1%, obtains just dry powder body;Wherein, it is dehydrated as follows no more than 1% concrete mode to water content: Calcium carbonate slurry dehydration is obtained by filtration in 200 mesh and is concentrated into water content no more than 25%, then stream is passed through with the speed of 1000kg/h Speed is 30m3It is atomized in/s, the air-flow that temperature is 380 DEG C, flash distillation to water content is not more than 1%;Activator be in mass ratio be 1: The palmitinic acid and lauric saponification liquor of 1-2 mixing;
(3) the first dry powder body of step (2) is not more than 0.1% through being dried to water content with dry machine, cooling, using 2 layers of paper Add 1 tunic packaging bag packaging can be obtained free from vacuum dehydrating can be used to production silane modified polyether seal glue calcium carbonate fill out Material.
Embodiment 3
The calcium carbonate that can be used to production silane modified polyether seal glue the present embodiment provides a kind of free from vacuum dehydrating is filled out Material, obtains by the following method:
(1) it is 40 μm of calcite in powder, water and Sodium Polyacrylate by diameter to mix according to the ratio that weight ratio is 1:1.5:0.1 Uniformly, adding diameter is the mill ball that 0.7-3.0mm accounts for three's weight 55%, and each size additional amount is 0.7- in mill ball The aluminium oxide ceramic ball 20% of 1.4mm, 1.4-2.0mm aluminium oxide ceramic ball 13%, 2.0-2.5mm aluminium oxide ceramic ball 14%, 2.5-3.0mm aluminium oxide ceramic ball 8%, being ground to calcium carbonate granule partial size is 0.5-4 μm, crosses 325 meshes and obtains calcium carbonate slurry Material;Grinding is by the way of stirring, mixing time 5h, mixing speed 6000r/min;
(2) activator for accounting for dry powder total weight 4% is added in calcium carbonate slurry, it is cooling in 80 DEG C of sufficiently reactions, then take off Water to water content is not more than 1%, obtains just dry powder body;Wherein, it is dehydrated as follows no more than 1% concrete mode to water content: will 325 mesh are obtained by filtration calcium carbonate slurry dehydration and are concentrated into water content no more than 25%, then are passed through flow velocity with the speed of 1800kg/h For 60m3It is atomized in/s, the air-flow that temperature is 450 DEG C, flash distillation to water content is not more than 1%;Activator be in mass ratio be 1:1 The saponification liquor of mixed stearic acid and palmitinic acid;
(3) the first dry powder body of step (2) is not more than 0.1% through being dried to water content with dry machine, cooling, using 2 layers of paper Add 1 tunic packaging bag packaging can be obtained free from vacuum dehydrating can be used to production silane modified polyether seal glue calcium carbonate fill out Material.
Although above the present invention is described in detail with a general description of the specific embodiments, On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.

Claims (7)

1. the pearl filler that a kind of free from vacuum dehydrating can be used to production silane modified polyether seal glue, which is characterized in that The pearl filler obtains by the following method:
(1) calcite raw material powder, water and grinding aid are mixed according to the ratio that weight ratio is 1:0.3-1.5:0.001-0.1 equal Even, adding diameter is the mill ball that 0.7-3.0mm accounts for three's weight 30-55%, and being ground to calcium carbonate granule partial size is 0.5-4 μm, it crosses 80-325 mesh and obtains calcium carbonate slurry;
(2) activator for accounting for dry powder total weight 0.5-4% is added in calcium carbonate slurry, it is cooling in 40-80 DEG C of sufficiently reaction, It is dehydrated again to water content no more than 1%, obtains just dry powder body;
(3) by the first dry powder body of step (2) through being dried to water content no more than 0.1% with dry machine, cooling adds 1 layer using 2 layers of paper Free from vacuum dehydrating, which can be obtained, in film package bag packaging can be used to the pearl filler of production silane modified polyether seal glue.
2. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that mill ball in the step (1) be alumina ball, zirconium aluminium ceramic ball, zirconia ball or One of Zirconium silicate ceramic ball.
3. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that in the step (2), be dehydrated as follows no more than 1% concrete mode to water content: by 80- The calcium carbonate slurry dehydration of 325 meshes is concentrated into water content no more than 25%, then is passed through flow velocity with the speed of 400-1800kg/h For 5-60m3In/s, the air-flow that temperature is 300-450 DEG C, flash distillation to water content is not more than 1%.
4. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that grinding aid is polyvinyl alcohol, Sodium Polyacrylate, polyphosphate sodium, sulfomethylated lignin in the step (1) One of sour sodium and silane coupling agent or their any combination.
5. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that the activator in the step (2) is one of C12~C22 fatty acid and C18 olefin(e) acid or two The saponification liquor of kind any of the above ratio mixing.
6. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that the calcite in powder of the selection in the step (1) is the calcite in powder that particle diameter is 15-40 μm.
7. the carbonic acid that a kind of free from vacuum dehydrating according to claim 1 can be used to production silane modified polyether seal glue Calcium filler, which is characterized in that the grinding in the step (1) is by the way of stirring, mixing time 1-5h, and mixing speed is 500-6000r/min。
CN201910247240.4A 2019-03-29 2019-03-29 A kind of free from vacuum dehydrating can be used to the pearl filler of production silane modified polyether seal glue Pending CN109825111A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256872A (en) * 2019-07-19 2019-09-20 良德纳米粉体创新科技(安徽)有限公司 Super fine calcium carbonate and its processing method

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CN104530768A (en) * 2014-12-26 2015-04-22 四川石棉巨丰粉体有限公司 Coarse whiting filler for gas-permeable membrane and preparation method of coarse whiting filler
CN104744971A (en) * 2015-03-04 2015-07-01 江西科越科技有限公司 Preparation process of wet-process superfine modified calcium carbonate
CN106674600A (en) * 2016-08-16 2017-05-17 四川云科微纳科技有限公司 Preparation method of chitosan-coated heavy calcium carbonate anti-microbial filler for breathable film
CN106893367A (en) * 2015-12-18 2017-06-27 池州灵芝化建材料科技有限公司 A kind of preparation method of modified superfine powdered whiting
CN108892975A (en) * 2018-08-03 2018-11-27 广西贺州市科隆粉体有限公司 A kind of preparation method of weather-proof powdered whiting

Patent Citations (6)

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Publication number Priority date Publication date Assignee Title
CN102977642A (en) * 2012-11-28 2013-03-20 东南新材料股份有限公司 Production method of superfine modified ground calcium carbonate by wet grinding
CN104530768A (en) * 2014-12-26 2015-04-22 四川石棉巨丰粉体有限公司 Coarse whiting filler for gas-permeable membrane and preparation method of coarse whiting filler
CN104744971A (en) * 2015-03-04 2015-07-01 江西科越科技有限公司 Preparation process of wet-process superfine modified calcium carbonate
CN106893367A (en) * 2015-12-18 2017-06-27 池州灵芝化建材料科技有限公司 A kind of preparation method of modified superfine powdered whiting
CN106674600A (en) * 2016-08-16 2017-05-17 四川云科微纳科技有限公司 Preparation method of chitosan-coated heavy calcium carbonate anti-microbial filler for breathable film
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256872A (en) * 2019-07-19 2019-09-20 良德纳米粉体创新科技(安徽)有限公司 Super fine calcium carbonate and its processing method

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