CN109400885A - A kind of preparation method of pectinate texture hydrophilic amino silicone oil - Google Patents
A kind of preparation method of pectinate texture hydrophilic amino silicone oil Download PDFInfo
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- CN109400885A CN109400885A CN201811174510.5A CN201811174510A CN109400885A CN 109400885 A CN109400885 A CN 109400885A CN 201811174510 A CN201811174510 A CN 201811174510A CN 109400885 A CN109400885 A CN 109400885A
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- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
The present invention relates to spinning post-finishing auxiliary agent technical fields, disclose a kind of preparation method of pectinate texture hydrophilic amino silicone oil.Intermediate tertiary amine groups polyethers is made in the present invention first, then, carries out quaternized and polymerization reaction with end epoxy silicon oil under the catalysis of organic acid, being made has regular pectinate texture, the equally distributed hydrophilic amino silicone oil of pendant polyether groups.Compared with the hydrophilic silicon oil prepared in the prior art, in the identical situation of hydrophily, fabric feeling more soft fluffy after being arranged with amido silicon oil prepared by the present invention, and technique according to the present invention is relatively simple, raw material is easy to get, reaction condition is relatively mild, is convenient for commercial applications and industrialization promotion.
Description
Technical field
The present invention relates to spinning post-finishing auxiliary agent technical field more particularly to a kind of pectinate texture hydrophilic amino silicone oils
Preparation method.
Background technique
With the improvement of living standards, more stringent requirements are proposed for snugness of fit of the people to fabric.Fabric of organosilicon
Post-finishing agent also requires the fabric after arranging to have certain hydrophily, no other than the fluffy feel of soft and smooth property to be met
Normal moisture absorption sweat discharging functions are influenced, this is particularly important to the value promotion of textile.
Hydrophilicrto polyether segment or quaternised modified to amino progress is introduced in the molecule, is to prepare hydrophilic amino silicon
Two kinds of common measures of oil.When the hydrophily to silicone oil is more demanding, need for both the above measure to be used in combination.It should infuse
Meaning, the distribution of quaternary ammonium salt group and polyether group in silicone molecule significantly affect the feel after arranging.In " hydrophilic ammonia
The synthesis and its application of base silicone oil ", Zhuan Baolu, printing and dyeing assistant, the 4th phase of volume 23 in April in 2006 one text, first prepare side chain
Then under the catalysis of organic acid tertiary amine compound is added, to introduce quaternary ammonium salt base in silicone oil with epoxy and polyether group
Group.Although the hydrophily of product is preferable, polyether group is dispensed directly on polysiloxanes segment, significantly affects polysiloxanes
The flexibility and film forming of segment cause the feel after arranging poor.In order to balance hydrophily and feel, need to polyether group
Distribution with quaternary ammonium salt group re-starts design, while meeting hydrophily requirement, minimizes polyether group to feel
Influence.
Summary of the invention
That in order to solve the above-mentioned technical problems, the present invention provides a kind of techniques is relatively simple, reaction condition is mild, can
Prepare that hydrophily is excellent and the method for the pectinate texture hydrophilic amino silicone oil of good hand touch.
The specific technical proposal of the invention is: a kind of preparation method of pectinate texture hydrophilic amino silicone oil, the amino
Silicone oil is the polymer being polymerized by raw material A, raw material B, raw material C and raw material D, and the raw material A is end containing hydrogen silicone oil, the original
Material B is allyl polyoxy alkyl epoxy base ether, and the raw material C is that allyl polyoxy alkyl epoxy base ether or allyl glycidyl are sweet
Oily ether, raw material D are N, N- dimethyl-N`- propyl -1,3- propane diamine or N, N- dimethyl-N`- ethyl -1,3- propane diamine；Amino
The preparation method of silicone oil the following steps are included:
(1) by raw material A, raw material B and solvent a addition system, after stirring is warming up to 60~80 DEG C, chloroplatinic acid catalyst is added,
After temperature is stablized, intermediate product 1: epoxy-terminated silicone oil is made in the reaction was continued 6~12h；
(2) raw material D, raw material C and solvent b are uniformly mixed, after stirring is warming up to 60~120 DEG C, react 6~12h, be made intermediate
Product 2: tertiary amine groups polyethers；
(3) organic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, reacts 8 after being warming up to 65~120 DEG C
Amido silicon oil is made in~16h.
The method and step that the present invention prepares pectinate texture hydrophilic amino silicone oil is relatively simple, and the pectinate texture parent prepared
Aqueous amido silicon oil, pendant polyether segment is distributed in uniform pectination, and on-position is on quaternary ammonium salt, to polysiloxane chain
The flexibility influence of section is smaller, and bi-quaternary ammonium salt structure has stronger cationic, has it in fabric fibre upper preferable
Oriented attachment ability and film forming.The hydrophily of pectinate texture hydrophilic amino silicone oil prepared by the present invention, feel and whiteness are equal
It meets the requirements, and technique is relatively simple, raw material is easy to get, and reaction condition is relatively mild, is convenient for commercial applications and industrialization promotion
The present invention need strict control prepare amido silicon oil various raw materials type, dosage and order of addition.The present inventor
Know, in above-mentioned formula, most of components has perhaps had the open raw material as hydrophilic silicon oil in the prior art,
But the present inventor wants, it is emphasized that creativeness of the invention is not merely for each one-component to be used as simple polymerization
Reaction, and be even more to be how to choose component the most suitable from the boundless and indistinct raw material of the prior art, and stringent match is carried out to it
Than limit, be made with target structure high molecular polymer so that the comprehensive performance of amido silicon oil reach most preferably with
Meet demand.This process needs to pay a large amount of creative work, and not need to only be tested by simple limited times can obtain
?.
The reason is that, choosing specific several from thousands of kinds of raw materials and limiting optimal proportion, this achievement is obtained
It needs to establish on the basis of a large amount of theory and practice.Further, team of the present invention finds in R&D process, amido silicon oil
Proportion setting between the selection and each component of raw material, the influence relationship between the comprehensive performance of amido silicon oil, by institute
Whiteness, hydrophily and the feel of the amido silicon oil to be considered are difficult to balance, and not show obviously regularity, often only
Micro-adjustment a certain kind raw material, order of addition or matching parameter, it is possible to a certain performance of amido silicon oil can be generated and have big shadow
It rings, such as hydrophily mixes up sometimes, but whiteness or feel are not inconsistent requirement suddenly simultaneously.Therefore research and development of the invention be
There is no an evident regularity guiding, there is certain " blindness " in the case where carry out, and since the present invention is each to amido silicon oil
The requirement of aspect performance is higher, therefore to obtain all good amido silicon oil of comprehensive performance, for common those skilled in the art
It is by no means easy for member.
Preferably, the mass ratio of the raw material A and raw material B are 100:1~10, the additional amount of solvent a in step (1)
It is zero or 0.2~0.25 times of raw material A quality, the mass volume ratio of raw material B and chloroplatinic acid is 160~240g:1mL.
When the mass ratio of raw material A and raw material B are 100:1~10, the macromolecule with the object of the invention structure can be obtained
Material.Raw material A and the mass ratio of raw material B have a very big impact the molecular structure of amido silicon oil, when the amount of raw material B is very few
When, raw material A reaction not exclusively, will continue to react, will be unable to after the double bond in raw material B is oxidized to epoxy group by chloroplatinic acid
To the macromolecule containing target structure.When the mass volume ratio of raw material B and chloroplatinic acid is 160~240g:1mL, can just it incite somebody to action
Double bond in raw material B is oxidized to epoxy group.
Preferably, the mass ratio of the material of the raw material D and raw material C are 1:1~1.05 in step (2)；Solvent b and original
The mass ratio for expecting C is 8~12:1.
The mass ratio of the material of raw material D and raw material C is 1:1~1.05, and the micro- excess of raw material C can guarantee finally obtained height
There is equally distributed branch in molecule, while can guarantee the quantity of branch.
Preferably, the mass ratio of the material of the intermediate product 1 and intermediate product 2 is 1:0.9~1.2 in step (3),
The mass ratio of raw material A is 0.8~2.4:100 in organic acid and step (1).
The mass ratio of the material of intermediate product 1 and intermediate product 2 is about 1:1, under proportion of the invention, can be had
The amount of the high molecular polymer of suitable molecular weight, intermediate product 2 it is excessive or it is very few can all cause to block, will be unable to obtain ideal poly-
Right high molecular material.
Preferably, the organic acid is at least one of acetic acid or lauric acid.
Preferably, the solvent a is isopropanol, solvent b is isopropanol, ethylene glycol monobutyl ether, ethylene glycol ether, second
The tertiary butyl ether of 2-ethoxyethanol, glycol monoethyl ether, ethylene glycol, diethylene glycol monomethyl ether, in dipropylene glycol and dipropylene glycol
At least one of monomethyl ether.
Preferably, the hydrogen content of the raw material A is 0.014~0.04%, the molecular weight of raw material B is 450~550g/
The molecular weight of mol, raw material C are 500~1200g/mol.
The restriction of the hydrogen content of raw material A end containing hydrogen silicone oil is particularly significant in the present invention, and hydrogen content determines in amido silicon oil
The length of polysiloxanes segment, the feel of fabric has a very big impact after arranging to amido silicon oil.Hydrogen content is higher, poly- silicon oxygen
The length of alkane segment is shorter, and specific gravity shared by polyether segment is bigger, and the hydrophily of the amido silicon oil of preparation is stronger, however whole with its
The feel of fabric after reason is poorer.On the contrary, hydrogen content is lower, the feel of the fabric after the amido silicon oil arrangement of preparation is better, so
And hydrophily is poorer.The present invention is to raw material B allyl polyoxy alkyl epoxy base ether and raw material C allyl polyoxy alkyl epoxy base
The molecular weight of ether or allyl glycidyl ether is defined respectively, the polyether chain segment length of amido silicon oil side chain of the invention
It spends longer, can guarantee hydrophilic while increasing main chain flexibility, be conducive to the hand for balancing fabric after amido silicon oil arranges
Sense and hydrophily.Using the raw material that limits of the present invention, available hydrophily and all good amido silicon oil of feel.
Preferably, the structural formula of the amido silicon oil are as follows:
Wherein, R1For CH2CH3Or CH2CH2CH3；
R2For
R3For
A is the integer between 5~40, and b is the integer between 0~20, and a` is the integer between 0~15, and b` is between 0~6
Integer, m are the integer between 50~500, and n is the integer between 5~50.
Branch flexible, main chain are evenly distributed on a kind of main chain of pectinate texture hydrophilic amino silicone oil of the invention
It is upper that there is hydrophilic polyether segment and quaternary ammonium salt group, it can guarantee amido silicon oil hydrophily with higher.Due to quaternary ammonium
The distribution of salt groups and polyether segment in silicone molecule has significant impact, therefore, this hair to the feel of fabric after arrangement
The position of both bright strict controls and the length of segment, hydrophily, whiteness and the feel of fabric after being arranged with balance.The prior art
In, it is difficult to meet the requirement of hydrophily, whiteness and feel simultaneously.
The present invention is that will gather by the benefit for designing the polyether segment design of different length in this way on main chain and side chain
Ether segment is dispersed in greatest extent on the strand of amido silicon oil, has the entire molecule of amido silicon oil all good hydrophilic
Property.The present invention designs the polyether segment on main chain at the both ends of polysiloxanes segment, and in polyether segment and polysiloxane chain
Section between short alkyl chain is set, caused by being directly connected directly with polysiloxanes segment to avoid polyether segment flexibility and at
The disadvantage of film property difference.Meanwhile the length of the polyether segment on amido silicon oil main chain is defined by the present invention, is guaranteeing its parent
Can have good feel and whiteness while aqueous.Quaternary ammonium salt group can be improved the whiteness of fabric, using epoxy group with
Tertiary amino is converted to quaternary ammonium salt group by tertiary amino reaction, and fabric is resistance to yellowing after raising arranges.Amido silicon oil of the invention
Pendant polyether segment in molecule is closely coupled with quaternary ammonium salt group, is not easy to be coated completely by polysiloxanes segment, can more fill
Synergistic effect between the two is waved in distribution, promotes the hydrophily of silicone oil；Its pendant polyether segment is distributed in uniform pectination, and is connect
Enter position on quaternary ammonium salt, smaller on the influence of the flexibility of polysiloxanes segment, bi-quaternary ammonium salt structure has stronger cation
Property, make it that there is upper preferable oriented attachment ability and film forming in fabric fibre.
Preferably, the structural formula of the raw material A are as follows:The structural formula of raw material B are as follows:The structural formula of allyl polyoxy alkyl epoxy base ether
Are as follows:Its structural formula of raw material D are as follows:
The present invention first reacts end containing hydrogen silicone oil with allyl polyoxy alkyl epoxy base ether, allyl polyoxy alkyl
The epoxy group of the end of epoxy group ether is reacted with end containing hydrogen silicone oil, by polysiloxanes segment and polyether segment R2Connection, and the two
Between have propoxyl group flexible.Therefore, in step (1), the poly- of both ends connection allyl polyoxy alkyl propoxyl group is formd
Siloxanes segment, then, end-allyl group is oxidized to epoxy terminated by chloroplatinic acid, obtains intermediate product 1 (epoxy-terminated silicone oil).So
Afterwards, the present invention is by allyl polyoxy alkyl epoxy base ether or allyl glycidyl ether and propyl -1 N, N- dimethyl-N`-,
The reaction of 3- propane diamine or the reaction of N, N- dimethyl-N`- ethyl -1,3- propane diamine, the active hydrogen in secondary amine are removed, in formation
Between product 2 (tertiary amine groups polyethers).Finally, organic acid and intermediate product 1 are added into intermediate product 2, the end of intermediate product 1 is utilized
Epoxy group is reacted with the tertiary amino in intermediate product 2, forms the polymer of amido silicon oil.
It is compared with the prior art, the beneficial effects of the present invention are: a kind of pectinate texture hydrophilic ammonia disclosed in the present invention
The preparation process of base silicone oil is relatively simple, and raw material is easy to get, and reaction condition is relatively mild, pushes away convenient for commercial applications and industrialization
Extensively.And amido silicon oil obtained has regular pectinate texture, pendant polyether groups are evenly distributed in polysiloxanes segment
Both ends are connected with quaternary ammonium salt.Not only there is preferable hydrophily, and soft, resistance to yellowing good.
Specific embodiment
The present invention will be further described with reference to the examples below.Related device, connection structure in the present invention
And method, if being device well known in the art, connection structure and method without refering in particular to.
Embodiment 1
A kind of preparation method of pectinate texture hydrophilic amino silicone oil, comprising the following steps:
(1) by 100g hydrogen content be 0.04% end containing hydrogen silicone oil, 4.55g allyl glycidyl ether be added reaction system in,
Stirring is warming up to 70 DEG C, and 0.02mL chloroplatinic acid catalyst is added, and after temperature is stablized, intermediate product 1 is made in the reaction was continued 8h:
Epoxy-terminated silicone oil；
(2) by 2.88g N, N- dimethyl-N`- propyl -1,3- propane diamine, 10g molecular weight is the allyl polyoxy of 500g/mol
Alkyl epoxy base ether, 30g ethylene glycol tertbutyl ether and 50g isopropanol are uniformly mixed, and are warming up to 60 DEG C, react 8h, are made intermediate
Product 2: tertiary amine groups polyethers；
(3) 2.4g glacial acetic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, is warming up to 80 DEG C, reaction
Amido silicon oil is made in 10h.
Embodiment 2
A kind of preparation method of pectinate texture hydrophilic amino silicone oil, comprising the following steps:
(1) end containing hydrogen silicone oil, 10g allyl polyoxy alkyl epoxy base ether, 25g isopropanol that 100g hydrogen content is 0.02% are added
Entering in reaction system, stirring is warming up to 75 DEG C, 0.05mL chloroplatinic acid catalyst is added, after system is transparent, the reaction was continued 8h, system
Obtain intermediate product 1: epoxy-terminated silicone oil；
(2) by 1.44g N, N- dimethyl-N`- propyl -1,3- propane diamine, 5g molecular weight is the allyl polyoxy alkane of 500g/mol
Basic ring oxygen ether, 53g ethylene glycol monobutyl ether are uniformly mixed, and are warming up to 60 DEG C, react 8h, and intermediate product 2 is made: tertiary amine groups are poly-
Ether；
(3) 1.2g glacial acetic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, is warming up to 80 DEG C, reaction
Amido silicon oil is made in 12h.
Embodiment 3
A kind of preparation method of pectinate texture hydrophilic amino silicone oil, comprising the following steps:
(1) by 100g hydrogen content be 0.014% end containing hydrogen silicone oil, 1.6g allyl glycidyl ether be added reaction system in,
Stirring is warming up to 80 DEG C, and 0.01mL chloroplatinic acid catalyst is added, and after system is transparent, intermediate product 1 is made in the reaction was continued 8h:
Epoxy-terminated silicone oil；
(2) by 1.01g N, N- dimethyl-N`- propyl -1,3- propane diamine, the allyl that 8.4g molecular weight is 1200g/mol is poly-
Oxyalkyl epoxy group ether, 74g ethylene glycol monobutyl ether are uniformly mixed, and are warming up to 60 DEG C, react 8h, and intermediate product 2: tertiary amine groups is made
Polyethers；
(3) 0.85g glacial acetic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, is warming up to 110 DEG C, reaction
Amido silicon oil is made in 12h.
Embodiment 4
A kind of preparation method of pectinate texture hydrophilic amino silicone oil, comprising the following steps:
(1) end containing hydrogen silicone oil, 10g allyl polyoxy alkyl epoxy base ether, 23g isopropanol that 100g hydrogen content is 0.02% are added
Entering in reaction system, stirring is warming up to 75 DEG C, 0.05mL chloroplatinic acid catalyst is added, after system is transparent, the reaction was continued 8h, system
Obtain intermediate product 1: epoxy-terminated silicone oil；
(2) by 1.44g N, N- dimethyl-N`- propyl -1,3- propane diamine, 5g molecular weight is the allyl polyoxy of 1200g/mol
Alkyl epoxy base ether, 53g ethylene glycol monobutyl ether are uniformly mixed, and are warming up to 90 DEG C, react 6h, and intermediate product 2 is made: tertiary amine groups are poly-
Ether；
(3) 1.2g glacial acetic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, is warming up to 120 DEG C, reaction
Amido silicon oil is made in 8h.
Comparative example
A kind of preparation method of pectinate texture hydrophilic amino silicone oil the following steps are included:
It is 0.05% side chain containing hydrogen silicone oil, 2.28g allyl glycidyl ether by 100g hydrogen content, 15g molecular weight is 500g/
The allyl polyoxy alkyl epoxy base ether of mol, 25g isopropanol are warming up to 70 DEG C or so, and chloroplatinic acid catalyst is added, saturating to system
Bright subsequent continuation of insurance temperature 8h；Then 4.26g dodeca-tertiary amine and 1.2g glacial acetic acid is added, is warming up to 80 DEG C of reaction 12h, amino silicone is made
Oil.
It is tested for the property using amido silicon oil made from Examples 1 to 4 and comparative example.Test method are as follows: by embodiment 1
~4 and comparative example made from amido silicon oil product stirred evenly with a small amount of nonionic emulsifier, then while stirring slowly plus water,
It is diluted to the lotion that silicone oil is 10wt%, finally with glacial acetic acid tune pH to 6 or so, finishing agent is made.With arrangement obtained
Agent handles all-cotton knitting cloth, dosage 30g/L, an immersing and rolling (pick-up: 70%) → drying and shaping (180 DEG C × 90S) → cold
But resurgence → performance evaluation.
Performance test is compared with: feel: touching rating method using more manpowers, is divided into 1~5 grade, the bigger numerical value the more soft；It is white
Degree: being measured by whiteness instrument, smaller with the difference of original cloth, illustrates that yellowing resistance is better；Hydrophily: water is dripped with standard dropper
In fabric surface, the time required for water droplet is permeated in fabric surface complete wetting is observed, the time is shorter, illustrates that hydrophily is got over
It is good.Test result is as shown in table 1
Table 1
| Sample serial number | Feel rank | Whiteness | Hydrophily |
| Original cloth | 1 | 94.3 | 0.5s |
| Embodiment 1 | 4 | 85.6 | 2.4s |
| Embodiment 2 | 4 | 87.4 | 1.8s |
| Embodiment 3 | 5 | 89.3 | 3.1s |
| Embodiment 4 | 5 | 89.5 | 1.5s |
| Comparative example | 2.5 | 87.8 | 1.6s |
By data in table 1 as it can be seen that amido silicon oil obtained can significantly improve the feel of original cloth by means of the present invention, make original
Cloth soft-touch, while the fabric after arrangement has certain hydrophily, does not influence normal moisture absorption sweat discharging functions, balances whole
The hydrophily, whiteness and feel of fabric after reason.Embodiment 4 is highly preferred embodiment of the present invention, with Examples 1 to 3 and comparative example
Compared to as it can be seen that the proportion between the selection and each component of raw materials and reagents type is set, between amido silicon oil comprehensive performance
Influence relationship, by being difficult to balance between the amido silicon oil performance to be considered, not show it is obviously regular,
Often micro-adjustment a certain kind component or matching parameter or order of addition, it is possible to a certain performance of amido silicon oil can be generated
Tool is big to be influenced.For example, feel and whiteness mix up sometimes, but hydrophily is not inconsistent requirement suddenly simultaneously.Therefore of the invention
Research and development be no evident regularity guiding, there is certain " blindness " in the case where carry out, and since the present invention is to ammonia
The requirement of base silicone oil various aspects of performance is higher, therefore to obtain all good amido silicon oil of comprehensive performance, for common ability
It is by no means easy for field technique personnel.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent structure transformation to the above embodiments, still fall within skill of the present invention
The protection scope of art scheme.
Claims (9)
1. a kind of preparation method of pectinate texture hydrophilic amino silicone oil, it is characterised in that: the amido silicon oil be by raw material A,
The polymer that raw material B, raw material C and raw material D are polymerized, the raw material A are end containing hydrogen silicone oil, and the raw material B is poly- for allyl
Oxyalkyl epoxy group ether, the raw material C are allyl polyoxy alkyl epoxy base ether or allyl glycidyl ether, and raw material D is
N, N- dimethyl-N`- propyl -1,3- propane diamine or N, N- dimethyl-N`- ethyl -1,3- propane diamine；The preparation side of amido silicon oil
Method the following steps are included:
(1) by raw material A, raw material B and solvent a addition system, after stirring is warming up to 60~80 DEG C, chloroplatinic acid catalyst is added,
After temperature is stablized, intermediate product 1: epoxy-terminated silicone oil is made in the reaction was continued 6~12h；
(2) raw material D, raw material C and solvent b are uniformly mixed, after stirring is warming up to 60~120 DEG C, react 6~12h, be made intermediate
Product 2: tertiary amine groups polyethers；
(3) organic acid and intermediate product 1 are successively added into intermediate product 2, stirs evenly, reacts 8 after being warming up to 65~120 DEG C
Amido silicon oil is made in~16h.
2. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: step
(1) in, the mass ratio of the raw material A and raw material B are 100:1~10, the additional amount of solvent a be zero or raw material A quality 0.2~
0.25 times, the mass volume ratio of raw material B and chloroplatinic acid is 160~240g:1mL.
3. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: step
(2) in, the mass ratio of the material of the raw material D and raw material C are 1:1~1.05；The mass ratio of solvent b and raw material C is 8~12:1.
4. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: step
(3) in, the mass ratio of the material of the intermediate product 1 and intermediate product 2 is 1:0.9~1.2, raw material A in organic acid and step (1)
Mass ratio be 0.8~2.4:100.
5. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as claimed in claim 4, it is characterised in that: described to have
Machine acid is at least one of acetic acid or lauric acid.
6. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: described molten
Agent a is isopropanol, and solvent b is isopropanol, ethylene glycol monobutyl ether, ethylene glycol ether, ethylene glycol monoethyl ether, ethylene glycol list first
The tertiary butyl ether of ether, ethylene glycol, diethylene glycol monomethyl ether, in dipropylene glycol and at least one of dipropylene glycol monomethyl ether.
7. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as claimed in claim 3, it is characterised in that: the original
The hydrogen content for expecting A is 0.014~0.04%, and the molecular weight of raw material B is 450~550g/mol, the molecular weight of raw material C is 500~
1200g/mol。
8. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: the ammonia
The structural formula of base silicone oil are as follows:
Wherein, R1For CH2CH3Or CH2CH2CH3；
R2For
R3For
A is the integer between 5~40, and b is the integer between 0~20, and a` is the integer between 0~15, and b` is between 0~6
Integer, m are the integer between 50~500, and n is the integer between 5~50.
9. a kind of preparation method of pectinate texture hydrophilic amino silicone oil as described in claim 1, it is characterised in that: the original
Expect the structural formula of A are as follows:The structural formula of raw material B are as follows:The structural formula of allyl polyoxy alkyl epoxy base ether
Are as follows:Its structural formula of raw material D are as follows:
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