CN102120893A - Modified talcpowder and preparation method thereof - Google Patents
Modified talcpowder and preparation method thereof Download PDFInfo
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- CN102120893A CN102120893A CN2010100338166A CN201010033816A CN102120893A CN 102120893 A CN102120893 A CN 102120893A CN 2010100338166 A CN2010100338166 A CN 2010100338166A CN 201010033816 A CN201010033816 A CN 201010033816A CN 102120893 A CN102120893 A CN 102120893A
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- properties
- correcting agent
- organosilicon
- copolyether
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Abstract
The invention relates to modified talcpowder and a preparation method thereof. The modified talcpowder comprises 100 mass parts of talcpowder and 0.5 to 2.5 mass parts of modifier, wherein the modifier is a mixture of polyalcohol laurate and organic silicon/polyether copolymer; the structural formula of the organic silicon/polyether copolymer is CH3(CH2)XC6H4(OC2H4)yO-Si(OCH3)2-CH2-CHR1R2; x is 5 to 15; y is 1 to 30; R1 is hydrogen, halogen or alkyl; and R2 is hydrogen, halogen or alkyl.
Description
Technical field
The present invention relates to a kind of modified talc powder, and the method for preparing modified talc powder.
Background technology
Talcum powder is a kind of mineral of being made up of the layered silicate crystal, and molecular formula is Mg
3[Si
4O
10] (OH)
2, there is hydrophilic radical on its surface, and is polarity, and the polymkeric substance majority has hydrophobicity, and consistency between the two is poor; Simultaneously, thin more talcum powder is easy to more in the course of processing reunite and finally influences the performance of filled polymer.Therefore, in order to improve interface combination between the two, must adopt appropriate means that talcum powder is carried out surface modification.
The method of modifying of using the coupling agent treatment filler is a kind of technology most widely used, with fastest developing speed.Usually contain a few class character group different with effect in the molecule of coupling agent, its function is the consistency of improving between filler and the polymkeric substance, fills the interaction between the component interface in the compound system thereby strengthen.The mechanism of modification is to utilize some small molecules that has amphiprotic group (oleophylic and hydrophilic radical) or macromolecular compound to carry out surface modification to carrying out in two kinds of materials of compound one or both, make its surface properties become hydrophilic by hydrophobic or become hydrophobicly by hydrophilic, purpose is to make two kinds of material combinations better.The kind of surface-modifying agent is a lot, different types of properties-correcting agent has different chemical property, and the surface modification of powder generally all has its specific Application Areas, its modified powder is made also difference to some extent of macromolecular material that filler is fit to and performance thereof, and, for improving modified effect and reducing the properties-correcting agent cost, also often cooperate complementation to carry out modification with multiple properties-correcting agent.
Patent CN1970647A discloses a kind of preparation method of composite modifier surface modified talcum powder, and this method is raw material with the talcum powder, adds properties-correcting agent talcum is carried out surface modification, and its technology is: take by weighing the talcum powder material, and in the high-speed mixer of packing into; Pre-thermal material makes material stir about 20min in the high-speed mixer high speed, controlled temperature≤90 ℃; Take by weighing diluent water, weight is by the KH-550 silane coupling agent: water is 1: 1~10; Take by weighing KH-550 silane coupling agent, sodium stearate, weight is pressed material: the KH-550 silane coupling agent: sodium stearate=100: 0.4~2.5: 0.5~2.0; Preparation duplex surface modification solution in the container of going into to be equipped with thinner, and stirs KH-550 silane coupling agent and sodium stearate; With surface modification solution slowly to going in the high-speed mixer, high-speed mixing 10~30min, controlled temperature≤100 ℃ promptly obtain the talcum powder of modification.This technology has modified effect preferably to talcum powder, but has added water in modifying process, needs after the modification talcum powder is carried out drying treatment, has increased operation and production cost.
Patent CN1673270A discloses a kind of polyvinyl chloride functional properties-correcting agent and preparation method thereof.This properties-correcting agent is by prescription acid polyol ester, Whitfield's ointment polyol ester, processing aids acrylic resin, oxidized homopolymer or oxidized polyethlene wax chemical combination to be formed.This properties-correcting agent has multiple functions such as coupling agent, dispersion agent, inside and outside lubricant agent, to PVC/CaCO
3Infill system has unique modifying function, can promote plasticizing, improve and disperse, improve and wear out and processing characteristics to have coupling enhancing and effect on thermal simultaneously, improve the physical and mechanical properties and the surface luster of goods, and can reduce part of auxiliary and use, reduce production costs.But this Technology Need raw material is more, and preparation process is comparatively complicated, causes the properties-correcting agent quality fluctuation easily.
Summary of the invention
The purpose of this invention is to provide a kind of modified talc powder and preparation method thereof.Described modified talc powder comprises the talcum powder of 100 mass parts and the properties-correcting agent of 0.5~2.5 mass parts, and properties-correcting agent is the mixture of lauric acid polyol ester and organosilicon/copolyether;
The lauric acid polyol ester can be one or more in lauric acid glycol ester, lauric acid propylene glycol ester, mono laurate glycerine ester, mono laurate butanediol ester, mono laurate trihydroxymethylpropanyl ester, the mono laurate pentaerythritol ester.
The structural formula of organosilicon/copolyether is:
CH
3(CH
2)
xC
6H
4(OC
2H
4)
yO-Si(OCH
3)
2-CH
2-CHR
1R
2
Wherein: x=5~15, preferred x=7~11; Y=1~30, preferred y=4~20; R
1Be hydrogen, halogen or alkyl; R
2Be hydrogen, halogen or alkyl.
Organosilicon/copolyether is for including (CH
2)
xC
6H
4(OC
2H
4)
yO-Si (OCH
3)
2The material of structural unit; Organosilicon/copolyether can be CH
3(CH
2)
8C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
3Or CH
3(CH
2)
8C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
2CH
3Or CH
3(CH
2)
7C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
2Cl or CH
3(CH
2)
11C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH (CH
3)
2In one or more.
Properties-correcting agent addition of the present invention is 0.5~2.5 part, is preferably 1.0~2.0 parts.
Lauric acid polyol ester content is 30%~60% in the properties-correcting agent of the present invention, and is preferred 30%~50%, and organosilicon/copolyether content is 40%~70%, preferred 50%~70%.
The preparation method of modified talc powder of the present invention is:
A. take by weighing dried talcum powder material, the Controllable Temperature of packing into is high mixes in the device;
B. take by weighing properties-correcting agent, mass ratio is pressed talcum powder: properties-correcting agent=100: 0.5~2.5;
C. the high-speed mixing material evenly adds the properties-correcting agent that is taken by weighing in the talcum powder of high mixed device, and stir 12min~25min under 80 ℃~120 ℃ temperature;
D. take out the talcum powder that obtains modification.
Lauric acid polyol ester in the properties-correcting agent can adopt commercially available product, for example the lauric acid propylene glycol ester of the good occasion chemical industry company limited in Shanghai; Also can adopt prior art to be prepared, be that the lauric acid polyol ester is obtained with polyvalent alcohol chemical combination such as propylene glycol or glycerine or butyleneglycol or tetramethylolmethanes by lauric acid: lauric acid is mixed with polyvalent alcohol, add catalyzer sodium hydroxide, heated and stirred, temperature is controlled at 180~210 ℃, reacts 3~5 hours, and reaction is finished, filter, get the lauric acid polyol ester.
Organosilicon in the properties-correcting agent/copolyether adopts prior art to be prepared: alkylphenol polyoxyethylene is mixed with organosilane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 110~120 ℃, react 10~11 hours, reaction is finished, add dry toluene, stirring and dissolving is removed insolubles, toluene is removed in underpressure distillation, obtains organosilicon/copolyether.
There is polar group on the talcum powder surface, and lauric acid polyol ester and organosilicon/copolyether all have polar group, can combine with the polar group on talcum powder surface preferably, improves modified effect.Modified talc powder of the present invention has very high settling volume and lower oil absorbency, can disperse preferably in matrix resin; Can be widely used in fields such as polypropylene, polyethylene, polyvinyl chloride and ABS.
Embodiment
For invention effect of the present invention is described, enumerate following examples, but the present invention is not limited in these embodiment.
1, analytical procedure
(1) measuring method of settling volume: take by weighing the 5.000g modified talc powder and place in the tool plug graduated cylinder of graduated 50mL, add certain amount of dispersant (whiteruss), after treating that modified talc powder is soaked into fully by whiteruss, add the scale of whiteruss again to 50mL, with the oscillation frequency of the 120 times/min 3min that fully vibrates, modified talc powder is uniformly dispersed in whiteruss, leaves standstill then, read the solid volume of different time.The settling volume of identical time can reflect the quality of consistency between particle and the organic solvent to a certain extent, and settling volume is big, illustrates that consistency is good.
(2) measuring method of oil number (with reference to " measuring method of YS/T618-2007 aluminium hydroxide used as filling material oil number "): get quantitative modified talc powder and put into watch-glass, dimixo-octyl phthalate is dripped by each 0.2mL, after each the dropping, fully grind with toolsetting, till can sticking into agglomerate and do not split to powder, oil number is with the volume V of every 100g sample institute oil suction
0(mL) expression is calculated as follows
In the formula, υ is the volume (mL) of the dimixo-octyl phthalate of consumption; M is the quality (g) of sample.Oil number has reflected the specific surface area of modified talc powder to a certain extent, and specific surface area is low more, and oil number is just low more, and wettability is just good more, and vice versa.
2, raw material sources
Talcum powder: the 1250 order products that Haicheng Jinghua Minerals Co., Ltd produces.
Lauric acid propylene glycol ester: the good occasion chemical industry company limited in Shanghai product.
The preparation of lauric acid polyol ester
The preparation of glyceryl monolaurate: the 200.0g lauric acid is mixed with 92.0g glycerine, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 200 ℃, react 4 hours, and reaction is finished, and filter, and get glyceryl monolaurate.
The preparation of mono laurate butanediol ester: with 200.0g lauric acid and 90.0g 1, the 2-butyleneglycol mixes, and adds catalyzer sodium hydroxide, and heated and stirred, temperature are controlled at 210 ℃, react 3 hours, and reaction is finished, and filters, and gets the mono laurate butanediol ester.
The preparation of mono laurate pentaerythritol ester: the 200.0g lauric acid is mixed with the 136.0g tetramethylolmethane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 180 ℃, react 5 hours, and reaction is finished, and filter, and get the mono laurate pentaerythritol ester.
The preparation of organosilicon/copolyether
The preparation of organosilicon/copolyether A: the 470.0g polyoxyethylene nonylphenol ether mixes with the 150.0g ethyl trimethoxy silane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 110 ℃, react 11 hours, reaction is finished, add dry toluene, stirring and dissolving is removed insolubles, toluene is removed in underpressure distillation, obtains organosilicon/copolyether A.
The preparation of organosilicon/copolyether B: the 200.0g polyoxyethylene octylphenol ether mixes with 164.0g n-propyl Trimethoxy silane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 110 ℃, react 10 hours, reaction is finished, add dry toluene, stirring and dissolving is removed insolubles, toluene is removed in underpressure distillation, obtains organosilicon/copolyether B.
The preparation of organosilicon/copolyether C: 300.0g dodecyl phenol polyethenoxy ether mixes with 198.5g γ-r-chloropropyl trimethoxyl silane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 115 ℃, react 11 hours, reaction is finished, add dry toluene, stirring and dissolving is removed insolubles, toluene is removed in underpressure distillation, obtains organosilicon/copolyether C.
The preparation of organosilicon/copolyether D: the 470.0g polyoxyethylene nonylphenol ether mixes with 178.0g isobutyl-Trimethoxy silane, add catalyzer sodium hydroxide, heated and stirred, temperature are controlled at 120 ℃, react 10 hours, reaction is finished, add dry toluene, stirring and dissolving is removed insolubles, toluene is removed in underpressure distillation, obtains organosilicon/copolyether D.
Embodiment 1
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent lauric acid propylene glycol ester 10.0g and organosilicon/copolyether A 10.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 100 ℃ temperature, stir 15min;
4) take out the talcum powder that obtains modification.
Embodiment 2
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent glyceryl monolaurate 4.0g and organosilicon/copolyether B 6.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 110 ℃ temperature, stir 20min;
4) take out the talcum powder that obtains modification.
Embodiment 3
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent glyceryl monolaurate 4.5g and organosilicon/copolyether C10.5g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 80 ℃ temperature, stir 25min;
4) take out the talcum powder that obtains modification.
Embodiment 4
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent lauric acid propylene glycol ester 9.0g and organosilicon/copolyether D 9.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 100 ℃ temperature, stir 12min;
4) take out the talcum powder that obtains modification.
Embodiment 5
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent lauric acid propylene glycol ester 6.0g, mono laurate butanediol ester 6.0g and organosilicon/oxygen ether copolymer B 8.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 120 ℃ temperature, stir 12min;
4) take out the talcum powder that obtains modification.
Embodiment 6
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent glyceryl monolaurate 10.0g, organosilicon/copolyether A 10.0g and organosilicon/copolyether C 5.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 100 ℃ temperature, stir 15min;
4) take out the talcum powder that obtains modification.
Embodiment 7
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent mono laurate butanediol ester 2.0g and organosilicon/copolyether B 8.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 90 ℃ temperature, stir 18min;
4) take out the talcum powder that obtains modification.
Embodiment 8
The talcum powder of modification prepares as follows:
1) take by weighing dried talcum powder material 1000g, the Controllable Temperature of packing into is high mixes in the device;
2) take by weighing properties-correcting agent mono laurate pentaerythritol ester 14.0g and organosilicon/copolyether C 6.0g;
3) properties-correcting agent that is taken by weighing is evenly added in the talcum powder of high mixed device, and under 110 ℃ temperature, stir 15min;
4) take out the talcum powder that obtains modification.
Comparative Examples 1
Described method is carried out according to embodiment 2, but properties-correcting agent changes glyceryl monolaurate 10g into.
Comparative Examples 2
Described method is carried out according to embodiment 3, but properties-correcting agent changes silane resin acceptor kh-550 (γ-propyl methacrylate base Trimethoxy silane) 15g into.
Comparative Examples 3
Described method is carried out according to embodiment 3, but properties-correcting agent changes titanate coupling agent NDZ-201[sec.-propyl three (dioctyl pyrophosphate) titanic acid ester into] 15g.
Settling volume and oil number to modified talc powder are tested, and the results are shown in Table 1.
The settling volume of table 1 modified talc powder and oil number test result
By embodiment 2 and Comparative Examples 1 as can be known, the settling volume of embodiment 2 is bigger under the identical time, and the oil number minimum illustrate that two kinds of properties-correcting agent are mixed uses has better surface modification effect.
By other embodiment and Comparative Examples as can be known, the settling volume of identical time is all big than Comparative Examples among the embodiment, and oil number all is lower than Comparative Examples, illustrate properties-correcting agent surface modification effect be better than silane resin acceptor kh-550 and titanate coupling agent NDZ-201.
Claims (9)
1. the talcum powder of a modification comprises the talcum powder of 100 mass parts and the properties-correcting agent of 0.5~2.5 mass parts, it is characterized in that properties-correcting agent is the mixture of lauric acid polyol ester and organosilicon/copolyether; The structural formula of organosilicon/copolyether is:
CH
3(CH
2)
xC
6H
4(OC
2H
4)
yO-Si(OCH
3)
2-CH
2-CHR
1R
2
Wherein: x=5~15; Y=1~30; R
1Be hydrogen, halogen or alkyl; R
2Be hydrogen, halogen or alkyl.
2. modified talc powder according to claim 1 is characterized in that comprising 1.0~2.0 parts of properties-correcting agent.
3. modified talc powder according to claim 1 is characterized in that lauric acid polyol ester content is 30%~60% in the properties-correcting agent; Organosilicon/copolyether content is 40%~70%.
4. modified talc powder according to claim 3 is characterized in that lauric acid polyol ester content is 30%~50% in the properties-correcting agent, and organosilicon/copolyether content is 50%~70%.
5. modified talc powder according to claim 1 is characterized in that lauric acid polyol ester in the properties-correcting agent is one or more in lauric acid glycol ester, lauric acid propylene glycol ester, mono laurate glycerine ester, mono laurate butanediol ester, mono laurate trihydroxymethylpropanyl ester, the mono laurate pentaerythritol ester.
6. modified talc powder according to claim 1 is characterized in that x is 7~11 in organosilicon/copolyether.
7. modified talc powder according to claim 1 is characterized in that y is 4~20 in organosilicon/copolyether.
8. modified talc powder according to claim 1 is characterized in that organosilicon/copolyether is CH
3(CH
2)
8C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
3, CH
3(CH
2)
8C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
2CH
3, CH
3(CH
2)
7C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH
2Cl, CH
3(CH
2)
11C
6H
4(OC
2H
4)
yOSi (OCH
3)
2CH
2CH (CH
3)
2In one or more.
9. the preparation method of the described modified talc powder of claim 1 is characterized in that the preparation method is:
A. take by weighing dried talcum powder material, the Controllable Temperature of packing into is high mixes in the device;
B. take by weighing properties-correcting agent, mass ratio is pressed talcum powder: properties-correcting agent=100: 0.5~2.5;
C. the high-speed mixing material evenly adds the properties-correcting agent that is taken by weighing in the talcum powder of high mixed device, and stir 12min~25min under 80 ℃~120 ℃ temperature;
D. take out the talcum powder that obtains modification.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108320839A (en) * | 2018-01-22 | 2018-07-24 | 雄智(上海)健身管理有限公司 | For fat-reducing wear, the elastomeric sensor conducting wire for clothing of reducing weight |
CN111748221A (en) * | 2020-07-07 | 2020-10-09 | 山东齐润源新材料科技有限公司 | Talcum powder granulation method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040091440A1 (en) * | 2002-11-08 | 2004-05-13 | Masanao Kamei | Hydrophilized powder and a composition comprising the same |
CN101151015A (en) * | 2005-03-31 | 2008-03-26 | 株式会社高丝 | Surface-coated powder and cosmetic preparation containing the same |
-
2010
- 2010-01-08 CN CN 201010033816 patent/CN102120893B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040091440A1 (en) * | 2002-11-08 | 2004-05-13 | Masanao Kamei | Hydrophilized powder and a composition comprising the same |
CN101151015A (en) * | 2005-03-31 | 2008-03-26 | 株式会社高丝 | Surface-coated powder and cosmetic preparation containing the same |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108320839A (en) * | 2018-01-22 | 2018-07-24 | 雄智(上海)健身管理有限公司 | For fat-reducing wear, the elastomeric sensor conducting wire for clothing of reducing weight |
CN111748221A (en) * | 2020-07-07 | 2020-10-09 | 山东齐润源新材料科技有限公司 | Talcum powder granulation method |
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