CN107459044A - A kind of inorganic agent for white carbon and preparation method thereof - Google Patents
A kind of inorganic agent for white carbon and preparation method thereof Download PDFInfo
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- CN107459044A CN107459044A CN201710612879.9A CN201710612879A CN107459044A CN 107459044 A CN107459044 A CN 107459044A CN 201710612879 A CN201710612879 A CN 201710612879A CN 107459044 A CN107459044 A CN 107459044A
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- inorganic agent
- white carbon
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- hydroxyl
- silicone oil
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 31
- 229920002545 silicone oil Polymers 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 14
- 229910000077 silane Inorganic materials 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 10
- 125000005389 trialkylsiloxy group Chemical group 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 239000004593 Epoxy Chemical group 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 6
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical group 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 abstract description 16
- 229920000570 polyether Polymers 0.000 abstract description 16
- 239000003921 oil Substances 0.000 abstract description 10
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 8
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 239000004964 aerogel Substances 0.000 description 11
- 230000002209 hydrophobic effect Effects 0.000 description 11
- 150000003384 small molecules Chemical class 0.000 description 9
- 150000003376 silicon Chemical class 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 4
- -1 polysiloxane Polymers 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 230000010148 water-pollination Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- QMMBZOSZCYBCDC-UHFFFAOYSA-N NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC Chemical compound NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC QMMBZOSZCYBCDC-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003254 anti-foaming effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- MDLRQEHNDJOFQN-UHFFFAOYSA-N methoxy(dimethyl)silicon Chemical compound CO[Si](C)C MDLRQEHNDJOFQN-UHFFFAOYSA-N 0.000 description 1
- XPDGHGYGTJOTBC-UHFFFAOYSA-N methoxy(methyl)silicon Chemical compound CO[Si]C XPDGHGYGTJOTBC-UHFFFAOYSA-N 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- GDYNEEHLNBYCLY-UHFFFAOYSA-N n'-[3-[methoxy(dimethyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(C)CCCNCCN GDYNEEHLNBYCLY-UHFFFAOYSA-N 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a kind of inorganic agent for white carbon, the inorganic agent can improve the compatibility between white carbon surface group and polyether modified silicon oil, suppress the generation of sedimentation, and then improve the outward appearance and application performance of defoamer, so as to reach the balance of superior defoaming and lasting suds.The present invention discloses a kind of preparation method of the inorganic agent for white carbon again, and step is few, and flow is simple, safe operation.
Description
Technical field
The present invention relates to technical field of organic chemistry, more particularly to a kind of inorganic agent and its preparation side for white carbon
Method.
Background technology
Defoamer can substantially be divided into the non-major class of silicon systems and silicon systems two according to the difference of main component.Non- silicon systems are to defoam
Agent mainly includes polyethers defoamer, mineral oil antifoam agent and higher alcohols defoamer；And the main component of silicon systems defoamer is then
Silicone oil, white carbon silicone oil cream or special modified silicon oil.Silicon systems defoamer is a kind of defoamer most widely used at present.
In modified silicon oil defoamer, polyether modified silicon oil is to apply and produce at present most one kind.Polyether-modified silicon
Oil is to introduce polyether siloxane copolymers made from polyether segment by hydrosilylation in siloxane molecule.Compared to
The polyethers obtained after simply silicone oil is mixed with polyethers and other auxiliary agents-silicone oil Compounded Antifoamer, find in practical application poly-
The suds ability of ethers defoamer is strong, but the relatively general polysiloxane-based defoamer of defoaming capacity is far short of what is expected.
In many application fields, such as papermaking, textile printing and dyeing, oil product processing, sewage disposal, oil exploitation and conveying, need
Defoamer is wanted to be provided simultaneously with good defoaming function and suds function.White carbon is added in polyether modified silicon oil to be greatly improved
Its antifoaming speed, optimize the suds balance that disappears.
But there is following defect in existing white carbon：It is anti-heavy in surname silicone oil system that existing white carbon changes in polyethers
Drop property is poor, it is easy to layering precipitation phenomenon occurs, influences the outward appearance and application performance of defoamer.
The content of the invention
For overcome the deficiencies in the prior art, an object of the present invention is to provide a kind of processing for white carbon
Agent, the modification agent can be modified to white carbon, affine between white carbon surface and polyether modified silicon oil to improve
Property, suppress the generation of sedimentation, and then improve the outward appearance and application performance of defoamer, so as to reach superior defoaming and persistently
The balance of suds.
The second object of the present invention is to provide a kind of preparation method of the inorganic agent for white carbon, and step is few, flow
Simply, safe operation.
An object of the present invention adopts the following technical scheme that realization：
A kind of inorganic agent for white carbon, the molecular structural formula of the inorganic agent is as shown in structural formula I：
Wherein, n=0-100；R is hydroxyl, carboxyl, epoxy radicals, hydrogen-based or the group for having reactivity with other silicone hydroxyls；
R1、R2、R3It is alkyl.
Further, n=10-50；R1、R2、R3It is methyl, ethyl or propyl group.
The second object of the present invention adopts the following technical scheme that realization：
A kind of preparation method of inorganic agent for white carbon, including：
Once add step：Hydroxyl three (trialkylsiloxy) silane monomer is added in reaction vessel；
Secondary addition step：Under conditions of nitrogen protection, difunctional silicone oil is added, is stirred；
Reactions steps：Add catalyst, temperature reaction；
Discharge step：Vacuumizing, reflux condensation mode, remove small molecule by-product, it is ensured that reaction carries out complete, cooling discharge,
Produce the inorganic agent.
Further, once added described in step, the molecular structure of hydroxyl three (trialkylsiloxy) silane monomer
Formula is as shown in structural formula II：
Wherein, X1、X2、X3It is methyl, ethyl or propyl group.
Further, in the secondary addition step, difunctional silicone oil and hydroxyl three (trialkylsiloxy) silane
The mol ratio of monomer is 1:1.
Further, in the secondary addition step, one end of the difunctional silicone oil carries silicone hydroxyl or silicon hydrogen
Base, the other end of the difunctional silicone oil is with blocking group or the hydroxyl without blocking group, carboxyl, epoxy radicals, hydrogen-based
Or other have the group of reactivity with silicone hydroxyl.
Further, in the reactions steps, 40-95 DEG C is warming up to, reacts 2-18h.
Further, in the reactions steps, the dosage of the catalyst is difunctional silicone oil and (three alkane of hydroxyl three
Base siloxy) silane monomer weight sum 0.01-2.0%.
Further, in the reactions steps, the catalyst is organic acid.
Further, the organic acid is one kind or any combination in acetic acid, caproic acid, octanoic acid, enanthic acid and chloroplatinic acid.
Compared with prior art, the beneficial effects of the present invention are：
(1) inorganic agent provided by the present invention for white carbon, white carbon surface base is improved by process of surface treatment
Compatibility between group and polyether modified silicon oil, suppresses the generation of sedimentation, and then improves the outward appearance and application performance of defoamer,
So as to reach the balance of superior defoaming and lasting suds.
(2) preparation method of the inorganic agent provided by the present invention for white carbon, step is few, and flow is simple, operation peace
Entirely.
Brief description of the drawings
Fig. 1 changes the mixed design sketch of surname silicone oil by the hydrophobic silicic aerogels that the embodiment of the present invention 1 provides with polyethers；
Fig. 2 changes the mixed design sketch of surname silicone oil by the hydrophobic silicic aerogels that comparative example 1 of the present invention provides with polyethers.
Embodiment
Below, with reference to accompanying drawing and embodiment, the present invention is described further, it is necessary to which explanation is, not
Under the premise of afoul, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
A kind of inorganic agent for white carbon, the molecular structural formula of inorganic agent is as shown in structural formula I：
Wherein, n=0-100, preferably 10-50；R be hydroxyl, carboxyl, epoxy radicals, hydrogen-based or other have instead with silicone hydroxyl
Answer the group of activity；R1、R2、R3It is alkyl, short hydrocarbon, preferably methyl, ethyl or propyl group.
A kind of preparation method of inorganic agent for white carbon, including：
Once add step：Hydroxyl three (trialkylsiloxy) silane monomer is added in reaction vessel；
Secondary addition step：Nitrogen protection under conditions of, add equimolar than difunctional silicone oil, stir；
Reactions steps：Add organic acid catalyst, temperature reaction；
Discharge step：Vacuumizing, reflux condensation mode, remove small molecule by-product, it is ensured that reaction carries out complete, cooling discharge,
Produce inorganic agent.
As further embodiment, in secondary addition step, one end of difunctional silicone oil with silicone hydroxyl or
Silicon hydrogen-based, the other end is with blocking group or the hydroxyl without blocking group, carboxyl, epoxy radicals, hydrogen-based or has instead with silicone hydroxyl
Answer the group of activity.
As further embodiment, in reactions steps, 40-95 DEG C is warming up to, reacts 2-18h；The use of catalyst
Measure the 0.01-2.0% for difunctional silicone oil and hydroxyl three (trialkylsiloxy) silane monomer weight sum；Catalyst is to have
Machine acid, preferably one kind or any combination in acetic acid, caproic acid, octanoic acid, enanthic acid and chloroplatinic acid.
This is used for the preparation flow of the inorganic agent of white carbon as shown in reaction equation I：
Wherein, X1、X2、X3It is methyl, ethyl or propyl group；Y is hydroxyl, carboxyl, epoxy radicals, hydrogen-based or other and silicon hydroxyl
Base has the group of reactivity, and Z is hydroxyl or hydrogen-based.
Hydroxyl three (trialkylsiloxy) silane monomer is added in reactor first, then in the condition of nitrogen protection
Under, add equimolar than difunctional silicone oil, stir；Organic acid catalyst is subsequently added into, is warming up to 40-95 DEG C, control
Reaction time processed is 2-18h, and during which, reactant carries out condensation reaction, generates target product and accessory substance；Finally vacuumize, return
Stream condensation, removes small molecule by-product, it is ensured that reaction progress is complete, cooling discharge, produces inorganic agent.
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained outside fixed by buying pattern.
Embodiment 1
A kind of inorganic agent for white carbon, its preparation method are as follows：
1st, (three silyloxies) silane body of hydroxyl three (structural formula III) is added in reaction vessel；
2nd, under nitrogen protection, add equimolar than both-end silicone hydroxyl silicone oil (structural formula IV), stir；
Wherein n=40；
3rd, the octanoic acid of total reactant weight 0.2% is added as catalyst, is warming up to 75 DEG C；
4th, vacuumize, reflux condensation mode 9h, remove small molecule product, it is ensured that reaction is carried out completely, and cooling discharge obtains white carbon
Inorganic agent.
The reaction process of embodiment 1 is as shown in reaction equation II：
Wherein, R1、R2、R3It is methyl, n=40.
The inorganic agent of above-mentioned acquisition is well mixed with hydrophily white carbon, adds 3- aminopropyl dimethyl methyl epoxide silicon
Alkane, 7h is reacted at 140 DEG C, vacuumize removing small molecule by-product, obtain hydrophobic silicic aerogels；Wherein, inorganic agent and 3- aminopropyls
The dosage of dimethyl methoxy silane is respectively the 10% and 1% of hydrophilic white carbon weight.
Embodiment 2
A kind of inorganic agent for white carbon, its preparation method are as follows：
1st, (three silyloxies) silane body of hydroxyl three (structural formula III) is added in reaction vessel；
2nd, under nitrogen protection, add equimolar than both-end containing hydrogen silicone oil (structural formula V), stir；
Wherein n=60；
3rd, the chloroplatinic acid of total reactant weight 0.01% is added as catalyst, is warming up to 55 DEG C；
4th, vacuumize, reflux condensation mode 9h, remove small molecule product, it is ensured that reaction is carried out completely, and cooling discharge obtains white carbon
Inorganic agent.
The reaction process of embodiment 2 is as shown in reaction equation III：
Wherein, R1、R2、R3It is methyl, n=60.
The inorganic agent of above-mentioned acquisition is well mixed with hydrophily white carbon, adds N- (β-aminoethyl)-γ-aminopropyl first
Base dimethoxysilane, 18h is reacted at 60 DEG C, vacuumize removing small molecule by-product, obtain hydrophobic silicic aerogels；Wherein, handle
The dosage of agent and N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane is respectively 30% He of hydrophilic white carbon weight
2%.
Embodiment 3
A kind of inorganic agent for white carbon, its preparation method are as follows：
1st, (three silyloxies) silane body of hydroxyl three (structural formula III) is added in reaction vessel；
2nd, under nitrogen protection, add equimolar than end alkoxy end hydroxyl silicone oil (structural formula VI), stir；
Wherein n=50；
3rd, the octanoic acid of total reactant weight 0.2% is added as catalyst, is warming up to 70 DEG C；
4th, vacuumize, reflux condensation mode 9h, remove small molecule product, it is ensured that reaction is carried out completely, and cooling discharge obtains white carbon
Inorganic agent.
The reaction process of embodiment 3 is as shown in reaction equation IV：
Wherein R1、R2、R3It is methyl, n=50.
The inorganic agent of above-mentioned acquisition is well mixed with hydrophily white carbon, adds N- (β-aminoethyl)-γ-aminopropyl two
Methylmethoxysilane, 10h is reacted at 200 DEG C, vacuumize removing small molecule by-product, obtain hydrophobic silicic aerogels；Wherein, handle
The dosage of agent and N- (β-aminoethyl)-γ-aminopropyl dimethyl methoxy silane is respectively 20% He of hydrophilic white carbon weight
0.5%.
Comparative example 1
300ml octamethylcy-clotetrasiloxanes are added in 500ml there-necked flask, under agitation, are slowly added into gas phase
White carbon, until mixture is in starchiness in flask, according to the amount of added white carbon, water is added in 4% ratio, at room temperature
1h is stirred, adds 10% HMDS, is incubated 2h；Caused ammonia in solvent and elimination reaction is steamed, is obtained
Hydrophobic silicic aerogels.
Effect assessment and performance detection
The hydrophobic silicic aerogels that Example 1-3 and comparative example 1 obtain, are added to same according to 5% addition respectively
In organosilicon modified polyether defoamer, room temperature is deposited 4 weeks, is observed delamination, is as a result seen Fig. 1 and Fig. 2.
Fig. 1 is the design sketch of embodiment 1, and Fig. 2 is the design sketch of comparative example 1.
It can be seen from figure 1 that the hydrophobic silicic aerogels of embodiment 1 and polyethers change after surname silicone oil system mixes, room temperature is placed 4 weeks
Afterwards without there is layering precipitation phenomenon, sample appearance is uniform, and this illustrates that the hydrophobic silicic aerogels resistance to settling of embodiment 1 can be good,
The outward appearance and application performance of defoamer are not interfered with.Embodiment 2-3 design sketch is close with embodiment 1, will not be repeated here.
As can be seen from Figure 2, the hydrophobic silicic aerogels of comparative example 1 and polyethers change after surname silicone oil system mixes, and room temperature is placed 4 weeks
After there is layering precipitation phenomenon, the hydrophobic silicic aerogels anti-settling poor performance of comparative example 1.
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (10)
1. a kind of inorganic agent for white carbon, it is characterised in that the molecular structural formula of the inorganic agent is as shown in structural formula I：
Wherein, n=0-100；R is hydroxyl, carboxyl, epoxy radicals or hydrogen-based；R1、R2、R3It is alkyl.
2. it is used for the inorganic agent of white carbon as claimed in claim 1, it is characterised in that n=10-50；R1、R2、R3It is first
Base, ethyl or propyl group.
A kind of 3. preparation method of the inorganic agent as claimed in claim 1 or 2 for white carbon, it is characterised in that including：
Once add step：Hydroxyl three (trialkylsiloxy) silane monomer is added in reaction vessel；
Secondary addition step：Under conditions of nitrogen protection, difunctional silicone oil is added, is stirred；
Reactions steps：Add catalyst, temperature reaction；
Discharge step：Vacuumize, reflux condensation mode, remove accessory substance, cooling discharge, produce the inorganic agent.
4. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that once add described
In step, the molecular structural formula of hydroxyl three (trialkylsiloxy) silane monomer is as shown in structural formula II：
Wherein, X1、X2、X3It is methyl, ethyl or propyl group.
5. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that in the secondary addition
In step, the mol ratio of difunctional silicone oil and hydroxyl three (trialkylsiloxy) silane monomer is 1:1.
6. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that in the secondary addition
In step, one end of the difunctional silicone oil carries silicone hydroxyl or silicon hydrogen-based, and the other end of the difunctional silicone oil carries
Hydroxyl, carboxyl, epoxy radicals or hydrogen-based.
7. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that in the reactions steps
In, 40-95 DEG C is warming up to, reacts 2-18h.
8. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that in the reactions steps
In, the dosage of the catalyst is difunctional silicone oil and hydroxyl three (trialkylsiloxy) silane monomer weight sum
0.01-2.0%.
9. it is used for the preparation method of the inorganic agent of white carbon as claimed in claim 3, it is characterised in that in the reactions steps
In, the catalyst is organic acid.
10. as claimed in claim 9 for white carbon inorganic agent preparation method, it is characterised in that the organic acid is
One kind or any combination in acetic acid, caproic acid, octanoic acid, enanthic acid and chloroplatinic acid.
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| CN201710612879.9A CN107459044B (en) | 2017-07-25 | 2017-07-25 | A kind of inorganic agent and preparation method thereof for white carbon |
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| CN201710612879.9A CN107459044B (en) | 2017-07-25 | 2017-07-25 | A kind of inorganic agent and preparation method thereof for white carbon |
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| CN107459044B CN107459044B (en) | 2018-08-10 |
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| CN107459044B (en) | 2018-08-10 |
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