CN111393654B - Preparation method of multifunctional nylon block silicone oil - Google Patents
Preparation method of multifunctional nylon block silicone oil Download PDFInfo
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- CN111393654B CN111393654B CN202010354755.7A CN202010354755A CN111393654B CN 111393654 B CN111393654 B CN 111393654B CN 202010354755 A CN202010354755 A CN 202010354755A CN 111393654 B CN111393654 B CN 111393654B
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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
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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
- D06M15/643—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
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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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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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
- D06M2101/34—Polyamides
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
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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
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the field of textile auxiliary agents, in particular to a preparation method of multifunctional block silicone oil for nylon. The epoxy resin is prepared by reacting epoxy-terminated silicone oil, amide polyether amine, isopropanol, tertiary amine polyether amine and glacial acetic acid. Polyether chain segments, polyamine chain segments, amide chain segments and quaternary amine chain segments are simultaneously introduced into the molecular structure of the silicone oil, and the finishing agent prepared from the multifunctional block silicone oil can endow the finished nylon fabric with excellent functions of softness, hydrophilicity, antibiosis, antistatic property and the like and water washing resistance.
Description
Technical Field
The invention relates to the field of textile auxiliary agents, in particular to a preparation method of nylon multifunctional block silicone oil.
Background
In recent years, amino polyether block silicone oil is developed rapidly in the textile industry, but is mainly synthesized by reacting epoxy-terminated silicone oil with ED series polyether amines (ED600, ED900 and ED2003), D series polyether amines (D150, D230 and D400) and tertiary amine series polyether amines, the finishing agent can endow the finished fabric with excellent soft hand feeling and provide certain hydrophilicity for the fabric, but the finishing agent has a small proportion of polyether chain segments in the structure, lacks polyamine chain segments, amide chain segments and quaternary amine chain segments, and often has the coexistence problem that the functions of softness, hydrophilicity, antibiosis, antistatic property and the like and the water washing resistance of the fabric cannot be better when the finishing agent is used for finishing nylon fabrics, so that the wearability is greatly reduced. Nylon fabric rigidity is great, and the grey cloth of weaving often is stiff, and to make the fabric after the finishing have soft, hydrophilic, antibiotic, antistatic function and resistant washing performance simultaneously, often need a plurality of finishing agent complex finishing, and numerous dye houses have accomplished the pipeline transportation at present, and a plurality of finishing agents use together means need more storage tank equipment, and this is unfavorable for the utilization of spatial position and the management of production prescription, and the manufacturing cost of dye house improves greatly.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of nylon multifunctional block silicone oil.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of multifunctional block silicone oil for nylon comprises the following steps:
adding 100 parts of epoxy-terminated silicone oil, 5-11 parts of amide polyether amine and 70-100 parts of isopropanol into a reaction container provided with a condensation reflux device, heating the reaction container to 80-83 ℃, carrying out heat preservation reaction for 5-8 hours, adding 7-14 parts of tertiary amine polyether amine and 1.5-3 parts of glacial acetic acid, and carrying out heat preservation reaction for 6-8 hours at 80-85 ℃ to obtain multifunctional block silicone oil, wherein the structural general formula is shown as follows;
wherein n is an integer of 45 to 80, x is an integer of 1 to 4, y is an integer of 7 to 11, z is an integer of 1 to 4, and a is an integer of 2 to 10.
Preferably, the structural general formula of the amide polyether amine is shown as follows;
wherein a is an integer of 2-10.
Preferably, the structural general formula of the tertiary amine polyether amine is shown as follows;
wherein x is an integer of 1 to 4, y is an integer of 7 to 11, and z is an integer of 1 to 4.
Due to the application of the technical scheme, the invention has the following advantages:
the self-made double-end epoxy amide polyether block silicone oil and tertiary amine polyether amine are catalyzed by glacial acetic acid to prepare multifunctional block silicone oil, a polyether chain segment with a high proportion is introduced into a silicone oil main chain, and after fibers are finished by the silicone oil, the polyether chain segment is exposed on the surfaces of the fibers, so that the hydrophilic capacity of the fibers is improved; the introduced amino chain segments are polyamine chain segments, the common advantages of the traditional block silicone oil and the traditional amino silicone oil are combined, and the fabric after finishing is endowed with excellent soft hand feeling; the structure of the introduced amide chain segment component is similar to that of a nylon fiber, and according to the principle of 'similar affinity and similar compatibility', the finishing agent can be intertwined with the fiber and crystallized together when baked, so that the finishing agent is anchored on the fiber, and the finished fabric has good water washing resistance; the silicone oil after quaternization has excellent antibacterial and antistatic properties, so that the problem that the silicone oil is soft, hydrophilic, antibacterial and antistatic functions and the water washing resistance of the silicone oil cannot well coexist when the silicone oil is used for finishing nylon fabrics is effectively solved, and the silicone oil has a good market prospect.
Detailed Description
The invention is further described below by means of specific embodiments.
Example 1: 100g of epoxy-terminated silicone oil with the number average molecular weight of 4000, 6.5g of amide polyether amine and 75g of isopropanol are added into a reaction container provided with a condensation reflux device, the temperature of the reaction container is raised to 81 ℃, the reaction is carried out for 6 hours under the condition of heat preservation, 8g of tertiary amine polyether amine and 1.8g of glacial acetic acid are added, and the reaction is carried out for 6 hours under the condition of heat preservation at 82 ℃, so that the multifunctional block silicone oil is prepared.
Example 2: adding 100g of epoxy-terminated silicone oil with the number average molecular weight of 5000, 7.5g of amide polyether amine and 80g of isopropanol into a reaction container with a condensation reflux device, heating the reaction container to 82 ℃, carrying out heat preservation reaction for 7 hours, adding 9g of tertiary amine polyether amine and 2g of glacial acetic acid, and carrying out heat preservation reaction for 7 hours at 83 ℃ to obtain the multifunctional block silicone oil.
Example 3: 100g of epoxy-terminated silicone oil with the number average molecular weight of 6000, 5.8g of amide polyether amine and 90g of isopropanol are added into a reaction vessel provided with a condensation reflux device, the temperature of the reaction vessel is raised to 83 ℃, the reaction is carried out for 8 hours under heat preservation, 7.5g of tertiary amine polyether amine and 1.6g of glacial acetic acid are added, and the reaction is carried out for 8 hours under heat preservation at 83 ℃, so that the multifunctional block silicone oil is prepared.
The application and finishing process of the multifunctional block silicone oil comprises the following steps:
1. preparing a multifunctional block silicone oil emulsion:
and (3) respectively and uniformly stirring the silicone oil products in the examples and the comparative examples with a small amount of a nonionic emulsifier, then adding water while stirring to obtain an emulsion with the solid content of 15%, and finally adjusting the pH value to 4-6 by using glacial acetic acid.
2. The finishing process comprises the following steps:
the fabric used was: nylon woven fabric.
The finishing process flow comprises the following steps: padding working solution (40 g/L of multifunctional block silicone oil emulsion, 60-70% of padding rate after one padding operation) → baking (195 ℃ C.. times.40 s-60 s) → cooling and moisture regaining for 24 hours → testing performance.
3. And (3) application performance testing:
evaluation of flexibility:
and (4) evaluating by a hand touch method, wherein a multi-person hand touch evaluation method is adopted, the evaluation is divided into 1-5 grades, and the larger the numerical value is, the softer the numerical value is.
(ii) evaluation of hydrophilicity:
the test is carried out with reference to AATCC 79-2010 bleached textile Water absorption.
Thirdly, antibacterial property evaluation:
reference is made to GB/T20944.3-2008 < evaluation of antibacterial properties of textiles section 3:
the flask method was shaken for the test.
Fourthly, antistatic property evaluation:
the finished fabric was equilibrated at 25 ℃ RH 30% for 24 hours and then at YG
(B) The 342D type fabric static tester tests the peak voltage and half-life period according to the standard.
The results of the flexibility and hydrophilicity application performance test of the multifunctional block silicone oil of the present invention and the comparative example silicone oil are shown in table 1:
TABLE 1 softness and hydrophilicity application performance test results of multifunctional Block Silicone oil and comparative example Silicone oil
As can be seen from Table 1, after the fabric finishing agent prepared from the multifunctional block silicone oil disclosed by the invention finishes the fabric, compared with the original fabric and the comparative example, the fabric is softer in hand feeling and more excellent in hydrophilicity, and after the fabric is washed for 5 times, the hand feeling and the hydrophilicity of the finished fabric are reduced to a certain extent but are still better than those of the original fabric and the comparative example.
The antibacterial performance test results of the multifunctional block silicone oil of the invention and the comparative silicone oil are shown in table 2:
TABLE 2 antibacterial property test results of multifunctional block silicone oil and comparative example silicone oil
As can be seen from Table 2, after the fabric finishing agent prepared from the multifunctional block silicone oil is used for finishing the fabric, the antibacterial rates of escherichia coli and staphylococcus aureus are higher than those of the original fabric and the comparative example.
The results of the antistatic properties test of the multifunctional block silicone oil of the present invention and the comparative example silicone oil are shown in table 3:
TABLE 3 antistatic Properties of multifunctional Block Silicone oils and comparative example Silicone oils
| Sample number | Peak voltage/V | Half life/s |
| Original cloth | 2865 | 82.53 |
| Example 1 | 693 | 2.13 |
| Example 2 | 684 | 1.57 |
| Example 3 | 732 | 2.68 |
| Comparative example | 1507 | 33.69 |
As can be seen from Table 3, after the fabric is finished by the fabric finishing agent prepared by the multifunctional block silicone oil, the peak voltage and the half-life period are lower than those of the original cloth and the comparative example.
Claims (3)
1. A preparation method of multifunctional block silicone oil for nylon is characterized by comprising the following steps:
adding 100 parts of epoxy-terminated silicone oil, 5-11 parts of amide polyether amine and 70-100 parts of isopropanol into a reaction container provided with a condensation reflux device, heating the reaction container to 80-83 ℃, carrying out heat preservation reaction for 5-8 hours, adding 7-14 parts of tertiary amine polyether amine and 1.5-3 parts of glacial acetic acid, and carrying out heat preservation reaction for 6-8 hours at 80-85 ℃ to obtain multifunctional block silicone oil, wherein the structural general formula is shown as follows;
wherein n is an integer of 45 to 80, x is an integer of 1 to 4, y is an integer of 7 to 11, z is an integer of 1 to 4, and a is an integer of 2 to 10.
2. The preparation method of the nylon multifunctional block silicone oil according to claim 1, characterized in that: the structural general formula of the amide polyether amine is shown as follows;
wherein a is an integer of 2-10.
3. The preparation method of the nylon multifunctional block silicone oil according to claim 1, characterized in that: the structural general formula of the tertiary amine polyether amine is shown as follows;
wherein x is an integer of 1 to 4, y is an integer of 7 to 11, and z is an integer of 1 to 4.
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| CN112832029A (en) * | 2021-03-01 | 2021-05-25 | 陕西工业职业技术学院 | A kind of preparation method of finishing agent for fabric softening finishing |
| CN113004530A (en) * | 2021-04-12 | 2021-06-22 | 江苏尼美达科技有限公司 | Multi-component copolymer block silicone oil and preparation method thereof |
| CN115109256A (en) * | 2021-12-29 | 2022-09-27 | 浙江传化功能新材料有限公司 | Preparation method of block silicone oil with high flash point and low solvent content |
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