CN111171267B - High-elasticity resin modified silicone oil and preparation method thereof - Google Patents
High-elasticity resin modified silicone oil and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
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- C08G18/3228—Polyamines acyclic
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- 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
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
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- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The invention discloses high-elasticity resin modified silicone oil, which relates to the field of fine chemical synthesis and has a main structural general formula,
wherein A is CH2CH2O, B are
R1Is CH2CH2CH2R is
m, n, p, z, x is an integer, x is more than or equal to 3 and less than or equal to 5, m is more than or equal to 2 and less than or equal to 4, n is more than or equal to 5 and less than or equal to 7, p is more than or equal to 105 and less than or equal to 145, and z is more than or equal to 2 and less than or equal to 4. By adopting the technical scheme, the high-elasticity resin modified silicone oil is developed mainly according to the principle that the polyurethane material has a soft-hard chain segment block structure and can endow the material with high elasticity, and the high-activity polyurea elastic resin with the soft-hard block structure is added on the basis of the organosilicon soft segment, so that the structure of the silicone oil modified silicone oil has a soft-hard chain segment, and the silicone oil modified silicone oil has a better treatment effect compared with other silicone oil in the aspect of fabric treatment.
Description
Technical Field
The invention relates to the field of fine chemical synthesis, and particularly relates to high-elasticity resin modified silicone oil and a preparation method thereof.
Background
The development of the polyether amino silicone oil reaches a highly mature stage in recent 10 years, and reaches a price meat fighting stage of an inventory market, so that the performance is difficult to increase in an alternative increment manner, and the polyether amino silicone oil only occupies the market share of a competitor through price fighting; because the block silicone oil is highly transparent and highly homogeneous in synthesis process, core raw materials and cost effect, enterprises are forced to innovate the structure of the silicone oil to improve the performance effect, so that the block silicone oil and the amino silicone oil can be effectively replaced to readjust the market competition pattern. In recent years, various concepts of block silicone oil are developed, namely five-element and six-element multi-copolymerization block silicone oil, polyurethane polyether block silicone oil, T-type structured hyperbranched silicone oil and the like, but the essential structure of the block silicone oil is not changed, and the ternary components of polyether, amino and organosilicon cores are not basically changed, so that the bulkiness, the smoothness and the softness of the textiles cannot be improved when the block silicone oil is used for treating the textiles.
Disclosure of Invention
The invention aims to provide high-elasticity resin modified silicone oil which can effectively improve the softness, fluffiness and smoothness of textiles.
The above object of the present invention is achieved by the following technical solutions: a high-elasticity resin modified silicone oil has a general structural formula,
wherein A is CH2CH2O, B are
R1Is CH2CH2CH2R is
m, n, p, z, x is an integer, x is more than or equal to 3 and less than or equal to 5, m is more than or equal to 2 and less than or equal to 4, n is more than or equal to 5 and less than or equal to 7, p is more than or equal to 105 and less than or equal to 145, and z is more than or equal to 2 and less than or equal to 4.
By adopting the technical scheme, the high-elasticity resin modified silicone oil is developed mainly according to the principle that the polyurethane material has a soft-hard chain segment block structure and can endow the material with high elasticity, and the high-activity polyurea elastic resin with the soft-hard block structure is added on the basis of the organosilicon soft segment, so that the structure of the silicone oil modified silicone oil has a soft-hard chain segment, and the silicone oil modified silicone oil has a better treatment effect compared with other silicone oil in the aspect of fabric treatment.
A preparation method of high-elasticity resin modified silicone oil comprises the following steps:
step (1), preparation of polyurethane prepolymer
S1, adding 30-60 parts of polyethylene glycol into the first reaction kettle, and heating to 50-70 ℃;
s2, dropwise adding 100-150 parts of diphenylmethane diisocyanate into the first reaction kettle, preserving heat for 2-3 hours, and cooling to below 40 ℃ to obtain a polyurethane prepolymer;
step (2), preparation of high-elasticity resin modified silicone oil
a. Adding 200 parts of the polyurethane prepolymer prepared in the step (1) and 46-63 parts of N, N-dimethyl-1, 3-propane diamine into a second reaction kettle, heating to 40-50 ℃, and preserving heat for 2-4 hours;
b. adding 1600-2100 parts of epoxy-terminated polyether silicone oil and 1000-1300 parts of isopropanol into a second reaction kettle, heating to 75-80 ℃, carrying out heat preservation reaction for 8-10 hours, and cooling to below 40 ℃ to obtain the high-elasticity resin modified silicone oil.
By adopting the technical scheme, the reaction formula of the modified silicone oil is mainly as follows:
the first step is as follows: preparation of polyurethane prepolymer
The second step is that: preparation of high-elasticity resin modified silicone oil
Wherein A is CH2CH2O, B are
R1Is CH2CH2CH2R is
m, n, p, z, x is an integer, x is more than or equal to 3 and less than or equal to 5, m is more than or equal to 2 and less than or equal to 4, n is more than or equal to 5 and less than or equal to 7, p is more than or equal to 105 and less than or equal to 145, z is more than or equal to 2 and less than or equal to 4
The high-elasticity modified silicone oil is prepared by preparing a polyurethane prepolymer through the reaction of isocyanate and hydroxyl, modifying polyurethane through the reaction of amino and isocyanate, and performing chain extension reaction with end epoxy polyether silicone oil.
Wherein, the temperature of the whole reaction step does not exceed 100 ℃, thereby effectively reducing the potential safety hazard and being suitable for large-scale production.
Preferably, the number average molecular weight of the polyethylene glycol is 150-200, and the number average molecular weight of the epoxy-terminated polyether silicone oil is 9000-12000.
By adopting the technical scheme, when the molecular weight of the polyethylene glycol is too large, the performance is deteriorated, and when the molecular weight of the polyethylene glycol is too small, the elasticity is poor. The epoxy-terminated polyether silicone oil has a molecular weight which is too large, and the obtained soft hand feeling and the looseness are slightly deficient, and when the molecular weight is too small, the hand feeling smoothness is deficient. It is preferable within this limitation. If the molecular weight is no longer in this range, the overall product properties will be far from what we want.
Preferably, diphenylmethane diisocyanate in S2 is added dropwise to polyethylene glycol via a constant pressure dropping funnel.
Through adopting above-mentioned technical scheme, utilize constant pressure dropping funnel dropwise add diphenylmethane diisocyanate, be favorable to controlling reaction rate like this to be favorable to avoiding local reaction rate too fast and influence the quality of product.
Preferably, the reactions of step (1) and step (2) are both carried out under the protection of nitrogen or inert gas.
By adopting the technical scheme, the protection is carried out by nitrogen or inert gas, so that the oxidation of the materials by air in the reaction process can be reduced, and the quality of the final product is caused.
Preferably, during the reaction in the step (1) and the step (2), the materials are continuously stirred by a stirrer.
By adopting the technical scheme, on one hand, the material is fully mixed in the reaction process, the uniformity and stability of the reaction are ensured, on the other hand, the heat dissipation in the reaction process is also facilitated, and the influence on the quality of the final product due to overhigh local temperature of the reaction is avoided.
Preferably, the top of the reaction kettle is provided with a condensation reflux device.
Through adopting above-mentioned technical scheme, can get off the material condensation that volatilize like this to both avoided the waste of material, guaranteed environmental protection again, also helped controlling the temperature and the pressure of reaction simultaneously, guaranteed the normal clear of reaction.
In conclusion, the beneficial technical effects of the invention are as follows:
1. the high-elasticity resin modified silicone oil has excellent film forming property
2. Compared with similar products in the market, the high-elasticity resin modified silicone oil obtained by the application has obvious advantages in aspects of bulkiness and resilience;
3. the high-elasticity resin modified silicone oil obtained by the application has self-emulsifying property, and is diluted by a high-speed dispersion machine without using an emulsifier; 4. the method has the advantages of simple process, easy control of reaction process and suitability for industrial production.
Drawings
FIG. 1 is a flow chart of a preparation process of high-elasticity resin modified silicone oil.
Detailed Description
The present invention is described in further detail below with reference to fig. 1.
Example one
(1) Adding 30 parts of polyethylene glycol (with the number average molecular weight of 150) into a reaction kettle provided with a thermometer, a stirrer and a condensation reflux, heating to 50 ℃, introducing nitrogen, slowly dripping 100 parts of diphenylmethane diisocyanate into the reaction kettle through a constant-pressure dropping funnel, preserving heat for 3 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the polyurethane prepolymer.
(2) Adding 200 parts of the obtained polyurethane prepolymer and 63 parts of N, N-dimethyl-1, 3-propane diamine into a reaction kettle provided with a thermometer, a stirrer and a condensation reflux, heating to 40 ℃, introducing nitrogen, keeping the temperature for 4 hours, adding 2080 parts of epoxy-terminated polyether silicone oil (with the number average molecular weight of 9000) and 1300 parts of isopropanol, heating to 75 ℃, keeping the temperature for reaction for 10 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the high-elasticity resin modified silicone oil.
Comparative example one:
the difference between this comparative example and example one is set forth in the selection of a polyethylene glycol having a number average molecular weight of 100.
Comparative example two:
the difference between this comparative example and the first example is shown in the fact that the number average molecular weight of the selected epoxy terminated polyether silicone oil is 8000.
Example two
(1) Adding 45 parts of polyethylene glycol (with the number average molecular weight of 200) into a reaction kettle provided with a thermometer, a stirrer and a condensation reflux, heating to 60 ℃, introducing nitrogen, slowly dripping 113 parts of diphenylmethane diisocyanate into the reaction kettle through a constant-pressure dropping funnel, preserving heat for 2.5 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the polyurethane prepolymer.
(2) Adding 200 parts of the obtained polyurethane prepolymer and 46 parts of N, N-dimethyl-1, 3-propane diamine into a reaction kettle provided with a thermometer, a stirrer and a condensation reflux, heating to 45 ℃, introducing nitrogen, keeping the temperature for 3 hours, adding 2000 parts of epoxy-terminated polyether silicone oil (with the number average molecular weight of 12000) and 1200 parts of isopropanol, heating to 80 ℃, keeping the temperature for reaction for 10 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the high-elasticity resin modified silicone oil.
EXAMPLE III
(1) Adding 60 parts of polyethylene glycol (with the number average molecular weight of 200) into a reaction kettle provided with a thermometer, a stirrer and a condensation reflux, heating to 70 ℃, introducing nitrogen, slowly dripping 150 parts of diphenylmethane diisocyanate into the reaction kettle through a constant-pressure dropping funnel, preserving heat for 2 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the polyurethane prepolymer.
(2) Adding 200 parts of the obtained polyurethane prepolymer and 46 parts of N, N-dimethyl-1, 3-propane diamine into a reaction kettle, heating to 50 ℃, introducing nitrogen, keeping the temperature for 2 hours, adding 1600 parts of epoxy-terminated polyether silicone oil (the number average molecular weight is 11000) and 1000 parts of isopropanol, heating to 80 ℃, keeping the temperature for reaction for 10 hours, cooling to below 40 ℃, and stopping introducing the nitrogen to obtain the high-elasticity resin modified silicone oil.
Comparative example three:
the difference between this comparative example and example three is set forth in the selection of a polyethylene glycol having a number average molecular weight of 250.
Comparative example four:
the difference between this comparative example and example three is described in that the number average molecular weight of the selected epoxy terminated polyether silicone oil is 13000.
The application and finishing process of the high-elasticity resin modified silicone oil comprises the following steps:
1. dilute opening process of high-elasticity resin modified silicone oil
100 parts of high-elasticity resin modified silicone oil
200 portions of water
Acetic acid 2 parts
Note: the parts used are parts by mass, and the fabric used is: flannel and terylene knitted fabrics;
2. finishing process
The finishing process flow comprises the following steps: padding working fluid (10 g/L of high-elasticity resin modified silicone oil emulsion, and the padding rate of 70%) → pre-baking (170 ℃ for 15-45 s) → moisture regain for 1h → evaluation;
3. application performance testing
And (3) evaluating hand feeling: and (4) evaluating by using a touch method, adopting a 1-5-point evaluation method, evaluating by 1 point at the worst and 5 points at the best, simultaneously evaluating by 5 persons, and taking an average value. The evaluation includes the contents: bulk, smoothness;
softness: according to GB/T18318 determination of the bending length of textiles and fabrics: a long strip-shaped sample is taken and placed on a platform, a ruler is pressed on the sample, and the long axis of the sample is parallel to the length direction of the ruler. The ruler and the sample move on the platform along the long axis direction simultaneously, so that the part of the sample extending out of the platform is suspended and bent under the dead weight. The extension 1/2 of the specimen is the bend length when the downward bent tip of the specimen touches a slope at 41.5 deg.C from the horizontal. The bending rigidity of the sample is calculated by the bending length and the mass per unit area;
(1) sample preparation: measuring each sample for 4 times by 6 blocks in the warp and weft directions of 25mm by 25mm, and taking an average value;
(2) calculating the bending rigidity:
G＝mC310-2
in the formula: g-bending stiffness per unit width, mN. cm;
m-mass per unit area of sample, g/m2；
C-average bending length of the specimen, cm.
Wherein the mass per unit area of the flannel is 400g/m2The mass per unit area of the terylene is 300g/m2；
(3) The rebound resilience: compressing the textile with the thickness of 10cm to 5cm, then removing the acting force, observing the thickness of the textile after 10s, and calculating the rebound rate;
the application performance test results of the high-elasticity resin modified silicone oil, the traditional block silicone oil KF-8997 and the traditional block silicone oil TF-438 are shown in the following table:
TABLE 1 results of testing application Properties of highly elastic resin-modified Silicone oil (pile fabrics)
TABLE 2 result of application Performance test of high elastic resin modified Silicone oil (Terylene Fabric)
Wherein, the traditional silicone oil KF-8997 can be purchased from Zhejiang Kong Silicone Co., Ltd, and the traditional block silicone oil TF-438 can be purchased from Mitsubishi chemical group Co., Ltd.
As can be seen from the results of the tests in tables 1 and 2, the modified silicone oils of examples 1 to 3 of the present application can effectively ensure higher softness, bulkiness, smoothness and elasticity of the textile, especially flannel and terylene, compared with the conventional silicone oils.
In addition, as can be seen from comparison of example one with comparative examples 1 and 2, when the number average molecular weight of polyethylene glycol is less than 150, it is liable to cause deterioration in elasticity of the textile, and when the number average molecular weight of epoxy terminated polyether silicone oil is less than 9000, it is liable to cause deterioration in smoothness of the textile; secondly, as can be seen from the comparison of example three with comparative example 3 and comparative example 4, when the number average molecular weight of the polyethylene glycol is more than 200, the bulkiness and softness of the textile are easily caused to be deteriorated, and when the number average molecular weight of the epoxy terminated polyether silicone oil is more than 12000, the smoothness of the textile is easily caused.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (7)
1. A high-elasticity resin modified silicone oil is characterized in that: the general formula of the structure is as follows,
wherein A is CH2CH2O, B are
R1Is CH2CH2CH2R is
m, n, p, z, x is an integer, x is more than or equal to 3 and less than or equal to 5, m is more than or equal to 2 and less than or equal to 4, n is more than or equal to 5 and less than or equal to 7, p is more than or equal to 105 and less than or equal to 145, and z is more than or equal to 2 and less than or equal to 4.
2. The method for preparing a highly elastic resin-modified silicone oil according to claim 1, wherein: the method comprises the following steps: step (1), preparation of polyurethane prepolymer
S1, adding 30-60 parts of polyethylene glycol into the first reaction kettle, and heating to 50-70 ℃;
s2, dropwise adding 100-150 parts of diphenylmethane diisocyanate into the first reaction kettle, preserving heat for 2-3 hours, and cooling to below 40 ℃ to obtain a polyurethane prepolymer;
step (2) preparation of high-elasticity resin modified silicone oil
a. Adding 200 parts of the polyurethane prepolymer prepared in the step (1) and 46-63 parts of N, N-dimethyl-1, 3-propane diamine into a second reaction kettle, heating to 40-50 ℃, and preserving heat for 2-4 hours;
b. and adding 1600-2100 parts of end epoxy polyether silicone oil and 1000-1300 parts of isopropanol into the second reaction kettle, heating to 75-80 ℃, carrying out heat preservation reaction for 8-10 hours, and cooling to below 40 ℃ to obtain the high-elasticity resin modified silicone oil.
3. The method for preparing high-elasticity resin-modified silicone oil according to claim 2, characterized in that: the number average molecular weight of the polyethylene glycol is 150-200, and the number average molecular weight of the epoxy-terminated polyether silicone oil is 9000-12000.
4. The method for preparing high elasticity resin modified silicone oil according to claim 2, wherein: in S2, the diphenylmethane diisocyanate was added dropwise to the polyethylene glycol via a constant pressure dropping hole.
5. The method for preparing high elasticity resin modified silicone oil according to claim 2, wherein: the reactions in the step (1) and the step (2) are carried out under the protection of nitrogen or inert gas.
6. The method for preparing high-elasticity resin-modified silicone oil according to claim 2, characterized in that: in the reaction process in the step (1) and the step (2), materials are continuously stirred by a stirrer.
7. The method for preparing high-elasticity resin-modified silicone oil according to claim 6, characterized in that: the top of the reaction kettle is provided with a condensing reflux device.
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| CN102660029A (en) * | 2012-05-04 | 2012-09-12 | 浙江润禾有机硅新材料有限公司 | Cation modified supersoft hydrophilic block silicone oil compound and preparation method and application |
| CN104628990A (en) * | 2015-02-27 | 2015-05-20 | 苏州大学 | Smooth and elastic silicone oil for textiles as well as preparation method and application of smooth and elastic silicone oil |
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| CN102660029A (en) * | 2012-05-04 | 2012-09-12 | 浙江润禾有机硅新材料有限公司 | Cation modified supersoft hydrophilic block silicone oil compound and preparation method and application |
| CN104628990A (en) * | 2015-02-27 | 2015-05-20 | 苏州大学 | Smooth and elastic silicone oil for textiles as well as preparation method and application of smooth and elastic silicone oil |
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