CN106622018A - Compound organosilicone surfactant - Google Patents
Compound organosilicone surfactant Download PDFInfo
- Publication number
- CN106622018A CN106622018A CN201611255600.8A CN201611255600A CN106622018A CN 106622018 A CN106622018 A CN 106622018A CN 201611255600 A CN201611255600 A CN 201611255600A CN 106622018 A CN106622018 A CN 106622018A
- Authority
- CN
- China
- Prior art keywords
- parts
- organic silicon
- silicon surfactant
- surfactant
- well mixed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/017—Mixtures of compounds
- C09K23/018—Mixtures of two or more different organic oxygen-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a compound organosilicone surfactant. The compound organosilicone surfactant is prepared from the following raw materials: a phosphate type organosilicone surfactant, a carboxyl polyether organosilicone surfactant, a polyether modified polysiloxane nonionic surfactant, sodium lauryl sulfate, nonylphenol polyoxyethylene ether, octaphenyl polyoxyethyiene ether, isomeric tridecanol fatty alcohol polyoxyethylene ether, octadecyl trimethyl ammonium chloride, cetyl trimethyl ammonium bromide, dodecyl dimethyl benzyl ammonium chloride, petroleum sodium sulfonate, sorbitan oleate and nonylphenol polyoxyethylene ether. The compound organosilicone surfactant disclosed by the invention has excellent surface activity and chemical stability, good emulsifying property and low surface tension.
Description
Technical field
The present invention relates to a kind of surfactant, more particularly to a kind of compound organic silicon surfactant.
Background technology
Surfactant, refers to the material for adding the interface state that can make its solution system on a small quantity that significant change occurs.Tool
There is fixed hydrophilic lipophilic group, align in the surface energy of solution.The molecular structure of surfactant has amphipathic：One
Hold as hydrophilic radical, the other end is hydrophobic grouping；Hydrophilic radical is often polar group, such as carboxylic acid, sulfonic acid, sulfuric acid, amino or amine
Base and its salt, hydroxyl, amide groups, ehter bond etc. also can be used as polar hydrophilic groups；And hydrophobic grouping is often nonpolar hydrocarbon chain, such as 8
Individual carbon atom above hydrocarbon chain.Surfactant is divided into ionic surfactant (including cationic surfactant and anion
Surfactant), nonionic surface active agent, amphoteric surfactant, compound surfactant, other surfaces activating agent
Deng.
In prior art, the demand when performance of single surfactant product cannot meet actually used, therefore urgently
A kind of compound organic silicon surfactant need to be designed to meet actual demand.
The content of the invention
To solve technical problem present in background technology, the present invention proposes a kind of compound organic silicon surfactant,
With excellent surface-active and chemical stability, with good emulsifiability, and surface tension is low.
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
Organic silicon surface active agent 5-15 parts, carboxylated polyther organic silicon surfactant 2-5 parts, Siloxane-Oxyalkylene Copolymers nonionic table
Face activating agent 15-25 parts, SDS 2-8 parts, NPE 3-6 parts, OPEO 4-8
Part, isomerous tridecanol AEO 2-5 parts, OTAC 3-6 parts, cetyl trimethyl bromine
Change ammonium 1-3 parts, dodecyl benzyl dimethyl ammonium chloride 4-8 parts, petroleum sodium sulfonate 3-6 parts, sorbitol anhydride oleate 4-8
Part, NPE 2-5 parts.
Preferably, the raw material of phosphate type organic silicon surfactant includes by weight：Containing hydrogen silicone oil 5-15 parts, allyl
Base polyoxyethylene poly-oxygen propylene aether 8-22 parts, chloroplatinic acid 4-8 parts, phosphorus pentoxide 2-6 parts.
Preferably, phosphate type organic silicon surfactant is prepared by following technique：By containing hydrogen silicone oil and pi-allyl
Polyoxyethylene poly-oxygen propylene aether is well mixed, and is passed through nitrogen, stirs 5-15min, then heats to 85-95 DEG C, is subsequently added into chlorine
Platinic acid, is continuously heating to 95-105 DEG C, is incubated 4-5h, then in 110-120 DEG C, low-boiling-point substance 25-35min is taken off under 55-65kPa,
It is cooled to room temperature and obtains material a, be then passed through nitrogen in material a, be heated to 50-60 DEG C, is subsequently added into phosphorus pentoxide and mixes
Close uniform, be continuously heating to 70-80 DEG C, be incubated 3-5h, be cooled to room temperature and obtain phosphate type organic silicon surfactant.
Preferably, in the raw material of phosphate type organic silicon surfactant, reactive hydrogen mass fraction is in containing hydrogen silicone oil
0.14-0.18%, viscosity is 143-3000mPas.
Preferably, in the raw material of phosphate type organic silicon surfactant, allyl polyethenoxy polyethenoxy ether it is flat
Molal weight is 1250-1500g/mol, and double bond content >=0.5mmol/g, hydroxyl value is 32-48mg/g, acid number≤0.3mg/g,
Its middle hydroxyl value and acid number are with KOH calculating.
Preferably, the raw material of polyether-modified surfactant includes by weight：Allyl alcohol 2-5 parts, oxirane 3-6
Part, expoxy propane 2-4 parts, chloromethanes 1-3 parts, octamethylcy-clotetrasiloxane 3-8 parts, containing hydrogen silicone oil 2-6 parts, the silica of hexamethyl two
Alkane 2-4 parts, potassium hydroxide 3-5 parts, sodium carbonate 4-8 parts, chloroplatinic acid 3-6 parts.
Preferably, the preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, under nitrogen protection, adds potassium hydroxide in fluid bed, then hangs potassium hydroxide stream of nitrogen gas increase
It is floating, it is subsequently added into sodium carbonate and water, and it is warming up to 120-130 DEG C, and 2-3h is dried, it is subsequently cooled to room temperature and obtains material a；
S2, in high-pressure reactor, allyl alcohol, oxirane and expoxy propane are well mixed, be warming up to 100-130
DEG C, 20-40min is incubated, 25-65 DEG C is then cooled to, add material a to be well mixed, then passing to chloromethanes carries out blocking instead
Should, hydrochloric acid neutralization is subsequently added into, after dehydration, it is filtrated to get material b；
S3, octamethylcy-clotetrasiloxane, containing hydrogen silicone oil and HMDO are well mixed, are warming up to 60-90 DEG C,
Insulation 3-5h, then proceedes to be warming up to 100-120 DEG C, is to deviate from unreacted small molecule under -0.9～-0.8MPa in vacuum,
It is cooled to room temperature and obtains material c, be then well mixed material c and material b, be warming up to 65-85 DEG C, be incubated 0.5-1.5h, connects
Addition chloroplatinic acid to be well mixed, be continuously heating to 90-100 DEG C, be incubated 20-40min, be cooled to room temperature and obtain polyether-modified poly-
Silicone nonionic surfactant.
Preferably, in the raw material of Siloxane-Oxyalkylene Copolymers nonionic surfactant, the matter of si-h bond in containing hydrogen silicone oil
Amount fraction is 0.18-0.19%.
Preferably, carboxylated polyther organic silicon surfactant：Number-average molecular weight Mn is 5000mg/mol, and carboxylic value is
1.327mmol/g, relative density d420 is 0.9860g/ml.
Preferably, phosphate type organic silicon surfactant, carboxylated polyther organic silicon surfactant and polyether-modified
The weight ratio of polysiloxane non-ionic surfactant is 8-12：3-4：18-22.
A kind of compound organic silicon surfactant of the present invention, its phosphoric acid ester type organosilicone surfactant
Agent, carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers nonionic surfactant, SDS,
NPE, OPEO, isomerous tridecanol AEO, octadecyl trimethyl chlorine
Change ammonium, cetyl trimethylammonium bromide, dodecyl benzyl dimethyl ammonium chloride, petroleum sodium sulfonate, sorbitan oleic acid
Ester and NPE.Wherein with phosphate type organic silicon surfactant and Siloxane-Oxyalkylene Copolymers nonionic table
Face activating agent be major ingredient, addition carboxylated polyther organic silicon surfactant, SDS, NPE,
OPEO, isomerous tridecanol AEO, OTAC, cetyl front three
Base ammonium bromide, dodecyl benzyl dimethyl ammonium chloride, petroleum sodium sulfonate, sorbitol anhydride oleate and Nonyl pheno
Ether is reinforcement material and auxiliary agent, wherein the phosphate type organic silicon surfactant for adding is with containing hydrogen silicone oil, allyl polyethenoxy
Polyethenoxy ether, chloroplatinic acid and phosphorus pentoxide are raw material, under the catalytic action of chloroplatinic acid, realize containing hydrogen silicone oil and pi-allyl
Polyoxyethylene poly-oxygen propylene aether hydrosilylation, then carries out esterification with phosphorus pentoxide, the phosphate for preparing
Type organic silicon surfactant has excellent surface-active and chemical stability, opens with good emulsifiability, and surface
Power is low.The Siloxane-Oxyalkylene Copolymers nonionic surfactant of addition with allyl alcohol, oxirane, expoxy propane, chloromethanes,
Octamethylcy-clotetrasiloxane, containing hydrogen silicone oil, HMDO, potassium hydroxide, sodium carbonate and chloroplatinic acid, with allyl alcohol as rise
Beginning agent, adds oxirane and expoxy propane, under the catalytic action of potassium hydroxide, adds sodium carbonate, is subsequently added into prestox
Cyclotetrasiloxane, containing hydrogen silicone oil and HMDO, in the presence of chloroplatinic acid catalyst, what is prepared is polyether-modified
Polysiloxane non-ionic surfactant has excellent surface-active and chemical stability, with good emulsifiability, and
Surface tension is low.The compound organic silicon surfactant of the present invention has excellent surface-active and chemical stability, has
Good emulsifiability, and surface tension is low.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this
It is bright, rather than for limiting the invention, any modification made on the basis of the present invention, equivalent etc. are at this
In bright protection domain.
In specific embodiment, the weight portion of phosphate type organic silicon surfactant can for 5 parts, 6 parts, 7 parts, 8 parts,
9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts；The weight portion of carboxylated polyther organic silicon surfactant can be 2
Part, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts；The weight portion of Siloxane-Oxyalkylene Copolymers nonionic surfactant can be with
For 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts；The weight portion of SDS
It can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts；The weight portion of NPE can for 3 parts, 3.5 parts, 4
Part, 4.5 parts, 5 parts, 5.5 parts, 6 parts；The weight portion of OPEO can for 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts,
6.5 parts, 7 parts, 7.5 parts, 8 parts；The weight portion of isomerous tridecanol AEO can for 2 parts, 2.5 parts, 3 parts, 3.5
Part, 4 parts, 4.5 parts, 5 parts；The weight portion of OTAC can for 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts,
5.5 parts, 6 parts；The weight portion of cetyl trimethylammonium bromide can be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts；Dodecyl
The weight portion of dimethyl benzyl ammonium chloride can be 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts；Stone
The weight portion of oily sodium sulfonate can be 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts；The weight of sorbitol anhydride oleate
Amount part can be 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts；The weight of NPE
Part can be 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts.
Embodiment 1
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
10 parts of organic silicon surface active agent, 3.5 parts of carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers non-ionic surface
20 parts of activating agent, 5 parts of SDS, 4.5 parts of NPE, 6 parts of OPEO, isomery 13
3.5 parts of alcohol AEO, 4.5 parts of OTAC, 2 parts of cetyl trimethylammonium bromide, ten
6 parts of dialkyl dimethyl benzyl ammonium chloride, 4.5 parts of petroleum sodium sulfonate, 6 parts of sorbitol anhydride oleate, Nonyl pheno
3.5 parts of ether.
Phosphate type organic silicon surfactant is prepared by following technique：By weight by 10 parts of containing hydrogen silicone oils and 15
Part allyl polyethenoxy polyethenoxy ether is well mixed, and is passed through nitrogen, stirs 10min, then heats to 90 DEG C, is subsequently added into
6 parts of chloroplatinic acids, are continuously heating to 100 DEG C, are incubated 4.5h, then in 115 DEG C, low-boiling-point substance 30min are taken off under 55-65kPa, are cooled to
Room temperature obtains material a, is then passed through nitrogen in material a, is heated to 55 DEG C, is subsequently added into 4 parts of phosphorus pentoxides and is well mixed,
75 DEG C are continuously heating to, 4h is incubated, room temperature are cooled to and are obtained phosphate type organic silicon surfactant.Wherein, in containing hydrogen silicone oil
Reactive hydrogen mass fraction is 0.16%, and viscosity is 285mPas.The average molar mass of allyl polyethenoxy polyethenoxy ether
For 1375g/mol, double bond content is 0.5mmol/g, and hydroxyl value is 40mg/g, and acid number is 0.3mg/g, its middle hydroxyl value and acid number with
KOH is calculated.
The preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, by weight under nitrogen protection, adds 4 parts of potassium hydroxide in fluid bed, then increases stream of nitrogen gas
Make potassium hydroxide suspend, be subsequently added into 6 parts of sodium carbonate and water, and be warming up to 125 DEG C, be dried 2.5h, be subsequently cooled to room temperature and obtain
To material a；
S2, in high-pressure reactor, 3.5 parts of allyl alcohols, 4.5 parts of oxirane and 3 parts of expoxy propane are well mixed, rise
Temperature is incubated 30min to 120 DEG C, is then cooled to 45 DEG C, adds material a to be well mixed, and then passes to 2 parts of chloromethanes and is sealed
End reaction, is subsequently added into hydrochloric acid neutralization, after dehydration, is filtrated to get material b；
S3,5.5 parts of octamethylcy-clotetrasiloxanes, 4 parts of containing hydrogen silicone oils and 3 parts of HMDOs are well mixed, are risen
Temperature is incubated 4h to 75 DEG C, then proceedes to be warming up to 110 DEG C, is to deviate from unreacted small molecule under -0.85MPa in vacuum, cold
But material c is obtained to room temperature, is then well mixed material c and material b, be warming up to 75 DEG C, be incubated 1h, be subsequently added into 4.5 parts
Chloroplatinic acid is well mixed, and is continuously heating to 95 DEG C, is incubated 30min, is cooled to room temperature and obtains Siloxane-Oxyalkylene Copolymers nonionic
Surfactant.
Wherein, the mass fraction of si-h bond is 0.185% in containing hydrogen silicone oil.Carboxylated polyther organic silicon surfactant：
Number-average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is 0.9860g/ml.
Embodiment 2
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
5 parts of organic silicon surface active agent, 5 parts of carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers non-ionic surface are lived
15 parts of agent of property, 8 parts of SDS, 3 parts of NPE, 8 parts of OPEO, isomerous tridecanol fat
2 parts of fat alcohol APEO, 6 parts of OTAC, 1 part of cetyl trimethylammonium bromide, dodecyl two
8 parts of methyl-benzyl ammonium chloride, 3 parts of petroleum sodium sulfonate, 8 parts of sorbitol anhydride oleate, 2 parts of NPE.
Phosphate type organic silicon surfactant is prepared by following technique：By weight by 5 parts of containing hydrogen silicone oils and 22
Part allyl polyethenoxy polyethenoxy ether is well mixed, and is passed through nitrogen, stirs 5min, then heats to 95 DEG C, is subsequently added into 4
Part chloroplatinic acid, is continuously heating to 105 DEG C, is incubated 4h, then in 120 DEG C, low-boiling-point substance 35min is taken off under 55kPa, is cooled to room temperature and obtains
To material a, then nitrogen is passed through in material a, is heated to 50 DEG C, be subsequently added into 6 parts of phosphorus pentoxides and be well mixed, continue to rise
Temperature is incubated 5h to 70 DEG C, is cooled to room temperature and obtains phosphate type organic silicon surfactant.Wherein, reactive hydrogen in containing hydrogen silicone oil
Mass fraction is 0.14%, and viscosity is 3000mPas.The average molar mass of allyl polyethenoxy polyethenoxy ether is
1250g/mol, double bond content 0.6mmol/g, hydroxyl value is 32mg/g, acid number 0.25mg/g, and its middle hydroxyl value and acid number are in terms of KOH
Calculate.
The preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, by weight under nitrogen protection, adds 3 parts of potassium hydroxide in fluid bed, then increases stream of nitrogen gas
Make potassium hydroxide suspend, be subsequently added into 8 parts of sodium carbonate and water, and be warming up to 120 DEG C, be dried 3h, be subsequently cooled to room temperature and obtain
Material a；
S2, in high-pressure reactor, 2 parts of allyl alcohols, 6 parts of oxirane and 2 parts of expoxy propane are well mixed, be warming up to
130 DEG C, 20min is incubated, is then cooled to 65 DEG C, add material a to be well mixed, then passing to 1 part of chloromethanes carries out blocking instead
Should, hydrochloric acid neutralization is subsequently added into, after dehydration, it is filtrated to get material b；
S3,8 parts of octamethylcy-clotetrasiloxanes, 2 parts of containing hydrogen silicone oils and 4 parts of HMDOs are well mixed, are heated up
To 60 DEG C, 5h is incubated, then proceedes to be warming up to 100 DEG C, be to deviate from unreacted small molecule under -0.8MPa in vacuum, cooled down
Material c is obtained to room temperature, is then well mixed material c and material b, be warming up to 65 DEG C, be incubated 1.5h, be subsequently added into 3 parts of chlorine
Platinic acid is well mixed, and is continuously heating to 100 DEG C, is incubated 20min, is cooled to room temperature and obtains Siloxane-Oxyalkylene Copolymers nonionic table
Face activating agent.
Wherein, the mass fraction of si-h bond is 0.18% in containing hydrogen silicone oil.Carboxylated polyther organic silicon surfactant：Number
Average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is 0.9860g/ml.
Embodiment 3
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
15 parts of organic silicon surface active agent, 2 parts of carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers non-ionic surface are lived
25 parts of agent of property, 2 parts of SDS, 6 parts of NPE, 4 parts of OPEO, isomerous tridecanol fat
5 parts of fat alcohol APEO, 3 parts of OTAC, 3 parts of cetyl trimethylammonium bromide, dodecyl two
4 parts of methyl-benzyl ammonium chloride, 6 parts of petroleum sodium sulfonate, 4 parts of sorbitol anhydride oleate, 5 parts of NPE.
Phosphate type organic silicon surfactant is prepared by following technique：By weight by 15 parts of containing hydrogen silicone oils and 8
Part allyl polyethenoxy polyethenoxy ether is well mixed, and is passed through nitrogen, stirs 15min, then heats to 85 DEG C, is subsequently added into
8 parts of chloroplatinic acids, are continuously heating to 95 DEG C, are incubated 5h, then in 110 DEG C, low-boiling-point substance 25min are taken off under 65kPa, are cooled to room temperature and obtain
To material a, then nitrogen is passed through in material a, is heated to 60 DEG C, be subsequently added into 2 parts of phosphorus pentoxides and be well mixed, continue to rise
Temperature is incubated 3h to 80 DEG C, is cooled to room temperature and obtains phosphate type organic silicon surfactant.Wherein, reactive hydrogen in containing hydrogen silicone oil
Mass fraction is 0.18%, and viscosity is 143mPas.The average molar mass of allyl polyethenoxy polyethenoxy ether is
1500g/mol, double bond content 0.7mmol/g, hydroxyl value is 48mg/g, acid number 0.28mg/g, and its middle hydroxyl value and acid number are in terms of KOH
Calculate.
The preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, by weight under nitrogen protection, adds 5 parts of potassium hydroxide in fluid bed, then increases stream of nitrogen gas
Make potassium hydroxide suspend, be subsequently added into 4 parts of sodium carbonate and water, and be warming up to 130 DEG C, be dried 2h, be subsequently cooled to room temperature and obtain
Material a；
S2, in high-pressure reactor, 5 parts of allyl alcohols, 3 parts of oxirane and 4 parts of expoxy propane are well mixed, be warming up to
100 DEG C, 40min is incubated, is then cooled to 25 DEG C, add material a to be well mixed, then passing to 3 parts of chloromethanes carries out blocking instead
Should, hydrochloric acid neutralization is subsequently added into, after dehydration, it is filtrated to get material b；
S3,3 parts of octamethylcy-clotetrasiloxanes, 6 parts of containing hydrogen silicone oils and 2 parts of HMDOs are well mixed, are heated up
To 90 DEG C, 3h is incubated, then proceedes to be warming up to 120 DEG C, be to deviate from unreacted small molecule under -0.9MPa in vacuum, cooled down
Material c is obtained to room temperature, is then well mixed material c and material b, be warming up to 85 DEG C, be incubated 0.5h, be subsequently added into 6 parts of chlorine
Platinic acid is well mixed, and is continuously heating to 90 DEG C, is incubated 40min, is cooled to room temperature and obtains Siloxane-Oxyalkylene Copolymers nonionic table
Face activating agent.
Wherein, the mass fraction of si-h bond is 0.19% in containing hydrogen silicone oil.Carboxylated polyther organic silicon surfactant：Number
Average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is 0.9860g/ml.
Embodiment 4
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
8 parts of organic silicon surface active agent, 4 parts of carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers non-ionic surface are lived
18 parts of agent of property, 7 parts of SDS, 4 parts of NPE, 7 parts of OPEO, isomerous tridecanol fat
3 parts of fat alcohol APEO, 5 parts of OTAC, 1.5 parts of cetyl trimethylammonium bromide, dodecyl
7 parts of dimethyl benzyl ammonium chloride, 4 parts of petroleum sodium sulfonate, 7 parts of sorbitol anhydride oleate, 3 parts of NPE.
Phosphate type organic silicon surfactant is prepared by following technique：By weight by 8 parts of containing hydrogen silicone oils and 20
Part allyl polyethenoxy polyethenoxy ether is well mixed, and is passed through nitrogen, stirs 8min, then heats to 92 DEG C, is subsequently added into 5
Part chloroplatinic acid, is continuously heating to 102 DEG C, is incubated 4.2h, then in 118 DEG C, low-boiling-point substance 32min is taken off under 58kPa, is cooled to room temperature
Material a is obtained, then nitrogen is passed through in material a, 52 DEG C are heated to, 5 parts of phosphorus pentoxides is subsequently added into and is well mixed, continued
72 DEG C are warming up to, 4.5h is incubated, room temperature are cooled to and are obtained phosphate type organic silicon surfactant.Wherein, it is living in containing hydrogen silicone oil
Property hydrogen mass fraction be 0.15%, viscosity is 3000mPas.The average molar mass of allyl polyethenoxy polyethenoxy ether
For 1254g/mol, double bond content 0.45mmol/g, hydroxyl value is 48mg/g, acid number 0.22mg/g, its middle hydroxyl value and acid number with
KOH is calculated.
The preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, by weight under nitrogen protection, adds 3.5 parts of potassium hydroxide in fluid bed, then increases stream of nitrogen gas
Ambassador's potassium hydroxide suspends, and is subsequently added into 7 parts of sodium carbonate and water, and is warming up to 122 DEG C, is dried 2.8h, is subsequently cooled to room temperature
Obtain material a；
S2, in high-pressure reactor, 3 parts of allyl alcohols, 5 parts of oxirane and 2.5 parts of expoxy propane are well mixed, heat up
To 125 DEG C, 25min is incubated, is then cooled to 62 DEG C, add material a to be well mixed, then passed to 1.5 parts of chloromethanes and sealed
End reaction, is subsequently added into hydrochloric acid neutralization, after dehydration, is filtrated to get material b；
S3,7 parts of octamethylcy-clotetrasiloxanes, 3 parts of containing hydrogen silicone oils and 3.5 parts of HMDOs are well mixed, are risen
Temperature is incubated 4.5h to 65 DEG C, then proceedes to be warming up to 105 DEG C, is to deviate from unreacted small molecule under -0.8MPa in vacuum,
It is cooled to room temperature and obtains material c, be then well mixed material c and material b, be warming up to 68 DEG C, be incubated 1.2h, is subsequently added into 4
Part chloroplatinic acid is well mixed, and is continuously heating to 98 DEG C, is incubated 25min, be cooled to room temperature obtain Siloxane-Oxyalkylene Copolymers it is non-from
Sub- surfactant.
Wherein, the mass fraction of si-h bond is 0.19% in containing hydrogen silicone oil.Carboxylated polyther organic silicon surfactant：Number
Average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is 0.9860g/ml.
Embodiment 5
A kind of compound organic silicon surfactant proposed by the present invention, its raw material includes by weight：Phosphate type has
12 parts of organic silicon surface active agent, 3 parts of carboxylated polyther organic silicon surfactant, Siloxane-Oxyalkylene Copolymers non-ionic surface are lived
22 parts of agent of property, 3 parts of SDS, 5 parts of NPE, 5 parts of OPEO, isomerous tridecanol fat
4 parts of fat alcohol APEO, 4 parts of OTAC, 2.5 parts of cetyl trimethylammonium bromide, dodecyl
5 parts of dimethyl benzyl ammonium chloride, 5 parts of petroleum sodium sulfonate, 5 parts of sorbitol anhydride oleate, 4 parts of NPE.
Phosphate type organic silicon surfactant is prepared by following technique：By weight by 12 parts of containing hydrogen silicone oils and 10
Part allyl polyethenoxy polyethenoxy ether is well mixed, and is passed through nitrogen, stirs 12min, then heats to 88 DEG C, is subsequently added into
7 parts of chloroplatinic acids, are continuously heating to 98 DEG C, are incubated 4.8h, then in 112 DEG C, low-boiling-point substance 28min are taken off under 62kPa, are cooled to room temperature
Material a is obtained, then nitrogen is passed through in material a, 58 DEG C are heated to, 3 parts of phosphorus pentoxides is subsequently added into and is well mixed, continued
78 DEG C are warming up to, 3.5h is incubated, room temperature are cooled to and are obtained phosphate type organic silicon surfactant.Wherein, it is living in containing hydrogen silicone oil
Property hydrogen mass fraction be 0.17%, viscosity is 143mPas.The average molar mass of allyl polyethenoxy polyethenoxy ether is
1495g/mol, double bond content 0.45mmol/g, hydroxyl value is 48mg/g, acid number 0.18mg/g, and its middle hydroxyl value and acid number are with KOH
Calculate.
The preparation method of Siloxane-Oxyalkylene Copolymers nonionic surfactant：Comprise the steps：
S1, by weight under nitrogen protection, adds 4.5 parts of potassium hydroxide in fluid bed, then increases stream of nitrogen gas
Ambassador's potassium hydroxide suspends, and is subsequently added into 5 parts of sodium carbonate and water, and is warming up to 128 DEG C, is dried 2.2h, is subsequently cooled to room temperature
Obtain material a；
S2, in high-pressure reactor, 4 parts of allyl alcohols, 4 parts of oxirane and 3.5 parts of expoxy propane are well mixed, heat up
To 105 DEG C, 35min is incubated, is then cooled to 28 DEG C, add material a to be well mixed, then passed to 2.5 parts of chloromethanes and sealed
End reaction, is subsequently added into hydrochloric acid neutralization, after dehydration, is filtrated to get material b；
S3,4 parts of octamethylcy-clotetrasiloxanes, 5 parts of containing hydrogen silicone oils and 2.5 parts of HMDOs are well mixed, are risen
Temperature is incubated 3.5h to 85 DEG C, then proceedes to be warming up to 115 DEG C, is to deviate from unreacted small molecule under -0.9MPa in vacuum,
It is cooled to room temperature and obtains material c, be then well mixed material c and material b, be warming up to 82 DEG C, be incubated 0.8h, is subsequently added into 5
Part chloroplatinic acid is well mixed, and is continuously heating to 92 DEG C, is incubated 35min, be cooled to room temperature obtain Siloxane-Oxyalkylene Copolymers it is non-from
Sub- surfactant.
Wherein, the mass fraction of si-h bond is 0.18% in containing hydrogen silicone oil.Carboxylated polyther organic silicon surfactant：Number
Average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is 0.9860g/ml.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (10)
1. a kind of compound organic silicon surfactant, it is characterised in that its raw material includes by weight：Phosphate type organosilicon
Surfactant 5-15 parts, carboxylated polyther organic silicon surfactant 2-5 parts, Siloxane-Oxyalkylene Copolymers non-ionic surface are lived
It is property agent 15-25 parts, SDS 2-8 parts, NPE 3-6 parts, OPEO 4-8 parts, different
Structure tridecanol AEO 2-5 parts, OTAC 3-6 parts, cetyl trimethylammonium bromide
1-3 parts, dodecyl benzyl dimethyl ammonium chloride 4-8 parts, petroleum sodium sulfonate 3-6 parts, sorbitol anhydride oleate 4-8 parts, nonyl
Base phenol polyethenoxy ether 2-5 parts.
2. compound organic silicon surfactant according to claim 1, it is characterised in that phosphate type organosilyl surface
The raw material of activating agent includes by weight：Containing hydrogen silicone oil 5-15 parts, allyl polyethenoxy polyethenoxy ether 8-22 parts, chloroplatinic acid
4-8 parts, phosphorus pentoxide 2-6 parts.
3. compound organic silicon surfactant according to claim 1 and 2, it is characterised in that phosphate type organosilicon
Surfactant is prepared by following technique：Containing hydrogen silicone oil and allyl polyethenoxy polyethenoxy ether are well mixed, are led to
Enter nitrogen, stir 5-15min, then heat to 85-95 DEG C, be subsequently added into chloroplatinic acid, be continuously heating to 95-105 DEG C, be incubated 4-
5h, then in 110-120 DEG C, takes off low-boiling-point substance 25-35min under 55-65kPa, be cooled to room temperature and obtain material a, then to material a
In be passed through nitrogen, be heated to 50-60 DEG C, be subsequently added into phosphorus pentoxide and be well mixed, be continuously heating to 70-80 DEG C, be incubated 3-
5h, is cooled to room temperature and obtains phosphate type organic silicon surfactant.
4. the compound organic silicon surfactant according to any one of claim 1-3, it is characterised in that phosphate type has
In the raw material of organic silicon surface active agent, reactive hydrogen mass fraction is 0.14-0.18% in containing hydrogen silicone oil, and viscosity is 143-
3000mPa·s。
5. the compound organic silicon surfactant according to any one of claim 1-4, it is characterised in that phosphate type has
In the raw material of organic silicon surface active agent, the average molar mass of allyl polyethenoxy polyethenoxy ether is 1250-1500g/
Mol, double bond content >=0.5mmol/g, hydroxyl value is 32-48mg/g, acid number≤0.3mg/g, and its middle hydroxyl value and acid number are in terms of KOH
Calculate.
6. the compound organic silicon surfactant according to any one of claim 1-5, it is characterised in that polyether-modified table
The raw material of face activating agent includes by weight：Allyl alcohol 2-5 parts, oxirane 3-6 parts, expoxy propane 2-4 parts, chloromethanes 1-3
Part, octamethylcy-clotetrasiloxane 3-8 parts, containing hydrogen silicone oil 2-6 parts, HMDO 2-4 parts, potassium hydroxide 3-5 parts, carbonic acid
Sodium 4-8 parts, chloroplatinic acid 3-6 parts.
7. the compound organic silicon surfactant according to any one of claim 1-6, it is characterised in that polyether-modified poly-
The preparation method of silicone nonionic surfactant：Comprise the steps：
S1, under nitrogen protection, adds potassium hydroxide in fluid bed, then makes potassium hydroxide suspend stream of nitrogen gas increase,
It is subsequently added into sodium carbonate and water, and is warming up to 120-130 DEG C, be dried 2-3h, is subsequently cooled to room temperature and obtains material a；
S2, in high-pressure reactor, allyl alcohol, oxirane and expoxy propane are well mixed, be warming up to 100-130 DEG C, protect
Warm 20-40min, is then cooled to 25-65 DEG C, adds material a to be well mixed, and then passing to chloromethanes carries out end capping reaction, connects
The neutralization of addition hydrochloric acid, after dehydration, material b is filtrated to get；
S3, octamethylcy-clotetrasiloxane, containing hydrogen silicone oil and HMDO are well mixed, are warming up to 60-90 DEG C, insulation
3-5h, then proceedes to be warming up to 100-120 DEG C, is to deviate from unreacted small molecule under -0.9～-0.8MPa in vacuum, cools down
Material c is obtained to room temperature, is then well mixed material c and material b, be warming up to 65-85 DEG C, be incubated 0.5-1.5h, then added
Enter chloroplatinic acid to be well mixed, be continuously heating to 90-100 DEG C, be incubated 20-40min, be cooled to room temperature and obtain polyether-modified poly- silica
Alkane nonionic surfactant.
8. the compound organic silicon surfactant according to any one of claim 1-7, it is characterised in that polyether-modified poly-
In the raw material of silicone nonionic surfactant, the mass fraction of si-h bond is 0.18-0.19% in containing hydrogen silicone oil.
9. the compound organic silicon surfactant according to any one of claim 1-8, it is characterised in that carboxylated polyther
Organic silicon surfactant：Number-average molecular weight Mn is 5000mg/mol, and carboxylic value is 1.327mmol/g, and relative density d420 is
0.9860g/ml。
10. the compound organic silicon surfactant according to any one of claim 1-9, it is characterised in that phosphate type
Organic silicon surfactant, carboxylated polyther organic silicon surfactant and Siloxane-Oxyalkylene Copolymers nonionic surfactant
Weight ratio be 8-12：3-4：18-22.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611255600.8A CN106622018A (en) | 2016-12-30 | 2016-12-30 | Compound organosilicone surfactant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611255600.8A CN106622018A (en) | 2016-12-30 | 2016-12-30 | Compound organosilicone surfactant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106622018A true CN106622018A (en) | 2017-05-10 |
Family
ID=58837596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611255600.8A Pending CN106622018A (en) | 2016-12-30 | 2016-12-30 | Compound organosilicone surfactant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106622018A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485278A (en) * | 2018-03-22 | 2018-09-04 | 广州冠道体育用品有限公司 | A kind of inner additive type antifogging agent composition for glasses |
| CN110745929A (en) * | 2019-10-17 | 2020-02-04 | 邱振权 | Emulsion flocculant |
| CN110982106A (en) * | 2019-12-27 | 2020-04-10 | 江苏美思德化学股份有限公司 | Organic silicon surfactant, soft polyurethane foam and preparation method thereof |
| CN111040188A (en) * | 2019-11-29 | 2020-04-21 | 湖北新四海化工股份有限公司 | Organic silicon emulsifier and preparation method thereof |
| CN111713493A (en) * | 2020-07-23 | 2020-09-29 | 陕西农塔生物数据研究有限公司 | Synergistic insecticidal auxiliary agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003018534A1 (en) * | 2001-08-23 | 2003-03-06 | Akzo Nobel Nv | A nitrogen-containing ortho ester-based surfactant, its preparation and use |
| CN103342818A (en) * | 2013-07-16 | 2013-10-09 | 扬州晨化科技集团有限公司 | Preparation method of polyether modified polysiloxane foam stabilizer |
| CN103820142A (en) * | 2014-02-28 | 2014-05-28 | 陕西省石油化工研究设计院 | Environment-friendly-type polluted oil processing agent |
-
2016
- 2016-12-30 CN CN201611255600.8A patent/CN106622018A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003018534A1 (en) * | 2001-08-23 | 2003-03-06 | Akzo Nobel Nv | A nitrogen-containing ortho ester-based surfactant, its preparation and use |
| CN103342818A (en) * | 2013-07-16 | 2013-10-09 | 扬州晨化科技集团有限公司 | Preparation method of polyether modified polysiloxane foam stabilizer |
| CN103820142A (en) * | 2014-02-28 | 2014-05-28 | 陕西省石油化工研究设计院 | Environment-friendly-type polluted oil processing agent |
Non-Patent Citations (1)
| Title |
|---|
| 黄良仙等: "磷酸酯型有机硅表面活性剂的制备及其表面活性", 《日用化学工业》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485278A (en) * | 2018-03-22 | 2018-09-04 | 广州冠道体育用品有限公司 | A kind of inner additive type antifogging agent composition for glasses |
| CN108485278B (en) * | 2018-03-22 | 2020-08-25 | 广州冠道体育用品有限公司 | Internal addition type antifogging agent composition for glasses |
| CN110745929A (en) * | 2019-10-17 | 2020-02-04 | 邱振权 | Emulsion flocculant |
| CN111040188A (en) * | 2019-11-29 | 2020-04-21 | 湖北新四海化工股份有限公司 | Organic silicon emulsifier and preparation method thereof |
| CN110982106A (en) * | 2019-12-27 | 2020-04-10 | 江苏美思德化学股份有限公司 | Organic silicon surfactant, soft polyurethane foam and preparation method thereof |
| CN111713493A (en) * | 2020-07-23 | 2020-09-29 | 陕西农塔生物数据研究有限公司 | Synergistic insecticidal auxiliary agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106622018A (en) | Compound organosilicone surfactant | |
| CN103182271B (en) | A kind of organic silicon surfactant and its preparation method and application | |
| CN105561634B (en) | Preparation method of defoaming agent resistant to high temperature and strong alkali | |
| CN103421324B (en) | Cross linking polysiloxane/acrylic ester compound emulsion and preparation method thereof and application | |
| KR19980032327A (en) | Method for preparing self-curing alkenyl hydride siloxane copolymer and coating composition | |
| TW200936644A (en) | Alkoxylated polyalkanolamines | |
| KR20120130289A (en) | Coating compositions with alkoxy-containing aminofunctional silicone resins | |
| CN102895805B (en) | The preparation method of non-silicon defoaming agent | |
| CN104844789B (en) | A kind of preparation method of polynary cooperative flame retardant polyalcohol and application | |
| TWI567136B (en) | The release sheet is an emulsion-stripping additive, an emulsified composition for a release sheet, and a release sheet | |
| CN105107237B (en) | A kind of organosilicon defoaming composition and preparation method thereof | |
| CN106693829A (en) | Modified composite type surface active agent | |
| JP5722451B2 (en) | Fully acylated amino-functional organopolysiloxane | |
| CN106492707A (en) | Surface activator composition | |
| CN107858002A (en) | A kind of shrinkage cable liquid silicon rubber composition and preparation method thereof | |
| KR20160113625A (en) | Organopolysiloxane compound and method for producing same, and addition-curable silicone composition | |
| CN106928267B (en) | The preparation method of quaternary trisiloxanes Gemini surface active agent | |
| CN110698691A (en) | Preparation method of hydrophobic amino silicone oil emulsion | |
| US20160096959A1 (en) | Curable silicone emulsion composition | |
| CN105040449B (en) | A kind of smoothing agent for fabric of organosilicon and preparation method thereof | |
| CN105295068A (en) | High-cation-degree asphalt emulsifier and application thereof | |
| CN103755946A (en) | Double-branch allylamine polyethenoxy ether and synthetic method thereof | |
| CN103804834A (en) | Organic silicon composition and preparation method thereof | |
| CN103073568B (en) | The preparation method of 1,3-diglycidyl ether epoxide propyl group-1,1,3,3 tetramethyl disiloxane | |
| CN105646565B (en) | A kind of synthesis of nitrile group-containing siloxanes and the preparation method of room temperature condensed type nitrile silicone rubber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170510 |
|
| WD01 | Invention patent application deemed withdrawn after publication |