CN112030551B - Finishing process of organic silicon fluoride-free waterproof soft polyester-based Raschel blanket - Google Patents
Finishing process of organic silicon fluoride-free waterproof soft polyester-based Raschel blanket Download PDFInfo
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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
- D06M15/6433—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing carboxylic groups
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- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
- D06M13/5135—Unsaturated compounds containing silicon atoms
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- 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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- 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
- D06M2200/12—Hydrophobic 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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Abstract
The invention relates to the technical field of blankets of textiles, in particular to a finishing process of an organic silicon fluorine-free waterproof soft terylene baschel blanket. Firstly, preparing an organic silicon fluorine-free waterproof soft finishing agent by a one-step in-situ polymerization method, and then using the organic silicon fluorine-free waterproof soft finishing agent for coating finishing of the polyester raschel blanket to obtain the organic silicon fluorine-free waterproof soft polyester raschel blanket. The finished raschel blanket has lasting waterproof, soft and wearability, and the organic silicon fluorine-free waterproof agent is environment-friendly and has simple production process, thereby improving the added value and market competitiveness of the terylene raschel blanket.
Description
Technical Field
The invention relates to the technical field of blankets of textiles, in particular to a finishing process of an organic silicon fluorine-free waterproof soft terylene baschel blanket.
Background
The raschel blanket has the advantages of bright color, good dyeing fastness, strong flower type main body feeling, soft fluff, comfortable hand feeling, good heat preservation performance, difficult deformation during washing and the like, is deeply loved by people, and is often used for high-grade blankets, high-grade cloth art toys, car decorations and the like. However, the conventional raschel blanket is usually a single-layer or multi-layer fabric, can only be covered on a body for keeping warm, does not have waterproof and moistureproof functions, and cannot meet the requirements of home textiles and outdoor use of people. Therefore, the development of a waterproof soft raschel blanket is very important.
Water repellents can impart hydrophobic properties to textile surfaces. Fluorine-containing water repellent is most widely used in the market. The fluorine-containing waterproof finishing agent can reduce the surface tension of the fabric to 10-15 mN/m, has excellent waterproof and oilproof effects, and the fabric finished by the fluorine-containing waterproof finishing agent has good hand feeling and excellent air permeability and moisture permeability. However, with the use of fluoropolymers in large quantities, the environmental problems associated with them have attracted considerable attention. The EU Perfluorooctylsulfonyl (PFOS) ban requires that PFOS or its related substances be present in the formulation at a level not exceeding 0.005% and in the semifinished product at a level not exceeding 0.1%, while PFOS is present in the textile or coating material at a level not exceeding 1 μ g/m 2 . As for perfluorooctanoic acid compounds (PFOA), it is also considered to have similar harmfulness to PFOS, and zero emission has been also demanded at present. Therefore, the development of a novel environment-friendly fluorine-free waterproof finishing agent and a finishing technology thereof plays a crucial role in improving the quality of the raschel blanket.
Along with the improvement of living standard and the upgrade of national industry, the textile printing and dyeing industry has more and more requirements on high-grade fluoride-free waterproof agents. However, the existing long aliphatic chain fluorine-free waterproof agent troubles dyeing and finishing enterprises, and mainly shows that after being finished by the waterproof agent, fabrics feel hard and the durability of the waterproof effect is poor. The hand feeling problem can be solved by using a softening agent together, but the waterproof performance is reduced; durability problems can be addressed by the use of cross-linking agents in combination or by increasing the amount of water repellent, but this can result in further reduction in the hand of the finished fabric. For example: european Jiansong CN 106632445B, a method for preparing an organosilicon waterproofing agent by using a hydrogen-containing silicone oil byproduct ] produces the organosilicon waterproofing agent by using the byproduct generated in the process of producing high-hydrogen-containing silicone oil, and develops a new technical processing route for producing the organosilicon waterproofing agent by using the byproduct. The branched polyamino long-chain alkyl polysiloxane and the waterproof soft organic silicon finishing agent are prepared by adopting a bulk polymerization mode, the branched polyamino long-chain alkyl polysiloxane and paraffin with a special melting point are mixed according to a certain proportion, and after heating, the mixed emulsifier is used for emulsification, so that the cationic organic silicon waterproof soft agent is obtained. The organic fluorine waterproof agent is used together with an organic fluorine waterproof agent and applied to nylon textiles. However, the above method does not involve molecular structure design of the water repellent, and the prepared water repellent has good water repellent effect and good hand feeling, but has poor washing resistance.
In recent years, the use of a specific molecular structure or the combination of a crosslinking agent has been the most effective way to improve the washing resistance of a water repellent. For example, dongfeng [ CN 110670343A, a cross-linking agent for improving washing fastness, its preparation method and waterproof fabric ] provides a cross-linking agent for improving washing fastness and its preparation method, the cross-linking agent can be matched with a waterproof agent to improve the washing fastness of the waterproof agent and prolong the service life of the waterproof fabric. Liujun CN 110452361A a synthesis method of a polyurethane acrylic acid modified organosilicon fluorine-free waterproof agent and a waterproof agent ] provides an organosilicon fluorine-free waterproof agent with excellent waterproofness and washing fastness, which is prepared by the synthesis of single-end aminoalkyl organosilicon and double-end hydroxyalkyl organosilicon, the synthesis of a polyurethane modified organosilicon macromonomer and the free radical emulsion polymerization of the macromonomer and adopts a special molecular structure. However, none of the above methods relate to the structural design and construction of a waterproof finish raschel blanket.
With the improvement of living standard and living quality, people have higher and higher requirements on the functionality of textiles. As an important textile, a carpet becomes a necessity for every family, and meanwhile, the functionality of people on the carpet is higher and higher. Among them, the waterproof function is a function that people pay attention to. The textile has a common property that the textile is easy to seep water. The textile used in some specific occasions needs to achieve the waterproof effect, and if the textile does not have the waterproof effect, the textile cannot play the role. Along with the continuous expansion of the use environment of the blanket, the blanket with the waterproof function can be favored by users.
The raschel blanket is made by taking acrylic fiber as a raw material, weaving the acrylic fiber by a raschel warp knitting machine, and performing cut-out, printing, finishing and sewing edge covering. Compared with other textiles, the advantages are outstanding: the Raschel blanket has the advantages of comfortable and soft hand feeling, fine and smooth fiber, no hair falling, heat preservation, ventilation, digital dyeing, bright color and no fading, and is thicker and more compact than a common blanket due to the unique process of the Raschel weaving method, and unique heat preservation performance. However, due to the characteristics of acrylic fibers, the current raschel blanket does not have a waterproof function.
The current fabrics including carpets are usually finished by waterproof finishing agents so as to have waterproof function. Most of the finishing agents for waterproof finishing of fabrics at present are fluorine-containing finishing agents.
The rise of fluorine-containing water repellent was in 1949, when a novel compound was synthesized by 3M company in the united states: perfluorooctyl sulfonic acid (PFOS) and a waterproof agent using the PFOS can generate a lotus effect on the surface of the clothes, and the clothes are not stained with water and oil, and are beautiful all the time in red. From this point on, fluorosurfactants have become the focus of development for various chemical companies.
The fluorine-containing compound has considerable harm, and the research and investigation of the environmental protection agency on PFOS shows that the fluorine-containing compound is one of the most difficult-to-decompose organic pollutants with extremely strong durability! Research results of research institutions in Europe, japan and China prove that the PFOS can be taken into organisms through various daily channels and is difficult to be discharged.
Therefore, from the viewpoint of environmental protection and health, it is necessary to finish fabrics such as carpets with a fluorine-free finishing agent.
Disclosure of Invention
The invention aims to provide a finishing process of an organic silicon fluoride-free waterproof soft polyester-based Raschel blanket, and relates to a finishing agent in the finishing process, wherein the finishing agent is environment-friendly, simple in production process and low in manufacturing cost, can be applied to industrial production of the Raschel blanket on a large scale, and the process can be used for preparing the organic silicon fluoride-free waterproof soft polyester-based Raschel blanket.
Specifically, the invention adopts the following technical scheme:
the application firstly provides a finishing process of an organic silicon fluorine-free waterproof soft terylene-based Raschel blanket, which comprises the following steps:
(1) Preparing an organic silicon fluoride-free waterproof soft finishing agent:
firstly, putting deionized water into a reaction kettle, then sequentially putting an organic silicon polymer, a surfactant, a catalyst and an initiator into the reaction kettle according to a proportion, and carrying out shearing emulsification to obtain an emulsion;
adjusting the temperature of the emulsion to 65-75 ℃ and 75-85 ℃, preserving the heat for 1-12h, and adjusting the pH value of the emulsion to 7 to obtain the organosilicon fluorine-free waterproof soft finishing agent;
(2) Pretreatment:
firstly, processing a polyester base Raschel blanket by adopting air plasma, then cleaning and drying after alkali decrement processing;
(3) Soft waterproof finishing:
firstly, diluting the finishing agent prepared in the step (1) and then preparing the diluted finishing agent and a cross-linking agent into coating finishing liquid;
then, putting the polyester-based Raschel blanket pretreated in the step (2) into the coating finishing liquid for soaking treatment, and carrying out two-soaking and two-rolling;
then, pre-baking at 100-120 ℃ for 5-10 min, baking at 150-190 ℃ for 1-5 min, taking out, and cooling to obtain the organic silicon fluorine-free waterproof soft-finished raschel blanket.
Preferably, the raw materials of the organosilicon fluorine-free waterproof soft finishing agent comprise the following components in parts by weight:
30-50% of organic silicon polymer, 1-5% of surfactant, 0.1-5% of catalyst, 0.1-2.5% of initiator and the balance of deionized water.
The content of water in the organosilicon fluorine-free soft waterproof finishing agent is increased or decreased according to needs, and the components are ensured to be emulsified.
Preferably, the organic silicon polymer comprises alkyl siloxane and modified silicone oil, and the weight ratio of the alkyl siloxane to the modified silicone oil is 4-6.
The distribution of the alkali decrement positions is the key of the method, and the uniform dispersion of the waterproof groups on the surface of the polyester fiber can be realized only by realizing the uniform distribution of the alkali decrement positions. To address this problem, the present inventors treated the polyester based raschel blanket with air plasma. The uniformity of the air plasma etching effect is better, and uniform etching points are formed on the surface of the terylene baschel blanket. The etching point can be used as a further alkali decrement positioning point of the terylene base Raschel blanket, so that the alkali decrement of the terylene base Raschel blanket is more regular and easy to control.
In the invention, the air plasma etching and alkali decrement treatment can also provide a storage place for the waterproof agent. In general, a key and difficult point in the functional finishing of textile fibers is the continuous distribution of the finishing agent in the fibers to be finished, so that the intended purpose can be well achieved. In the invention, through repeated experiments, the inventor finds that the pits and grooves on the surface of the polyester fiber in the polyester based raschel blanket subjected to alkali weight reduction treatment are completely filled, and the organic silicon fluorine-free waterproof softening finishing agent forms a continuous film on the surface of the polyester fiber, so that conditions are provided for good waterproofness and softness of the organic silicon fluorine-free waterproof flexible polyester raschel blanket.
The alkali liquor used for the alkali decrement of the polyester fiber is a sodium hydroxide solution or a potassium hydroxide solution, the alkality of the two solutions is strong, the polyester fiber is in the sodium hydroxide solution, ester bonds of polyester molecular chains on the surface of the fiber are hydrolyzed and broken, hydrolysis products with different polymerization degrees are continuously formed, and water-soluble sodium terephthalate and glycol are finally formed, so that the quality of the polyester fiber is lightened, the diameter of the fiber is thinned, the breaking strength is lowered, and the performance maintenance of the fabric is not facilitated. According to the structural characteristics of the terylene bashel blanket after air plasma etching and the particularity of the components of the terylene bashel blanket, the inventor screens mixed alkali with slightly weak alkalinity through a plurality of experiments as treatment liquid for alkali decrement, and can obtain a more ideal alkali decrement effect.
Preferably, the alkali solution in the alkali weight reduction treatment is obtained by mixing one of sodium hydroxide and potassium hydroxide with one of sodium bicarbonate, sodium carbonate, sodium phosphate and potassium carbonate in a mass ratio of 1.
Preferably, the mass concentration of the mixed alkali solution is 4-10 g/L; the temperature of the mixed alkali solution treatment is 80-90 ℃, and the time is 5-10 min.
Preferably, the alkylsiloxane is one or a mixture of more of octamethylcyclotetrasiloxane (D4), trifluoropropylmethylcyclotrisiloxane (D3F), tetramethyltetravinylcyclotetrasiloxane (D4V), methyltriethoxysilane (MTES), methyltrimethoxysilane (MTMS), phenyltriethoxysilane (KH-651), vinyltrimethoxysilane (KH-171), 3-methacryloxypropyltriethoxysilane (KH-571), γ -aminopropyltriethoxysilane (KH-550), γ - (2, 3 glycidoxy) propyltrimethoxysilane (KH-560).
Preferably, the modified silicone oil is one or a mixture of more of carboxyl silicone oil, amino silicone oil and epoxy modified silicone oil, the viscosity of the modified silicone oil is 200-1500 (Pa \8729s), and the number average molecular weight is 15000-30000.
Preferably, the alkylsiloxane is vinyltrimethoxysilane (KH-171); the modified silicone oil is carboxyl silicone oil, the viscosity is 1300 (Pa 8729s), and the number average molecular weight is 26000; the final composite is a silicone-carboxy silicone oil composite.
Preferably, the surfactant comprises MES (sodium fatty acid methyl ester sulfonate), DMSS (disodium coconut monoethanolamide sulfosuccinate) and CAB-35 (cocamidopropyl betaine), and the mass ratio of MES to DMSS to CAB-35 is 1-2.
Preferably, the mass ratio of MES, DMSS and CAB-35 is 1.
Preferably, the catalyst is one of DBSA (dodecyl benzene sulfonic acid), H2SO4 and HCl.
Preferably, the cross-linking agent is pentaerythritol-tri (3-aziridinyl) propionate and vinyl triethoxysilane, and the mass ratio of the pentaerythritol-tri (3-aziridinyl) propionate to the vinyl triethoxysilane is 3-6.
Preferably, the crosslinking agent is vinyltriethoxysilane. The water repellent contains vinyltriethoxysilane, which can effectively contact the fabric surface to form a silica three-dimensional network structure, so that water molecules and oil molecules are prevented from directly contacting the Raschel blanket. Meanwhile, the waterproof agent can fully permeate into the interior of the Raschel blanket, so that the waterproof performance is improved.
Preferably, the initiator comprises one or more of azobisisobutylamidine hydrochloride, azobisisobutylimidazoline hydrochloride, or ammonium persulfate.
Preferably, the concentration of the diluted organic silicon fluorine-free waterproof agent is 1-5%.
Preferably, the soaking time in the step (3) is 0.5-1 h; the padder pressure for the two-dipping and two-rolling is 0.3-0.5MPa.
Preferably, the air plasma etching treatment process comprises the following steps: a polyester-based raschel blanket suspended in a closed processing space, supplying a gas carbon dioxide for plasma etching into the closed space, and setting the pressure in the closed space to 5-20 Pa; the treatment time is 1-3min.
The invention is based on organosilicon fluorine-free water-repellent softening finishing agent, through the research and development of terylene-based Raschel blanket waterproof finishing technology, the environmental protection problem of the conventional long fluorine carbon chain fluorine-containing finishing agent (PFOA/PFOS) for finishing blanket fabrics is solved; meanwhile, the excellent water and oil repellent effect and hand feeling are kept. The polyester bas raschel blanket using the waterproof agent has the waterproof grade reaching 5 grade.
The invention has the beneficial effects that:
(1) The fluorine-free waterproof agent has the advantages of good waterproof performance, soft hand feeling, environmental friendliness, simple production process and low manufacturing cost, and can be applied to industrial production of fluorine-free waterproof Raschel blankets in a large scale.
(2) The water-based organic silicon fluorine-free waterproof agent is selected, the post-finishing process such as the soaking time of the finishing agent, the padder pressure of two-soaking and two-rolling, the pre-drying temperature and time and the like is systematically optimized, and the influence of the water-repellent effect and the hand feeling of the product is researched.
(3) The cross-linking agent is skillfully used, and a cross-linking network is constructed in the finishing process so as to improve the performances of the product, such as water resistance, rubbing fastness and the like.
Detailed Description
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
First, the present application prepared a silicone fluorine-free water repellent soft finish as specified in examples 1-3.
Example 1: an organic silicon fluoride-free waterproof soft finishing agent is prepared by the following specific steps:
putting 400g of deionized water into a reaction kettle, sequentially putting 100g of an organic silicon polymer (40 g of alkyl siloxane, 60g of modified silicone oil), 5g of a surfactant (MES: DMSS: CAB-35=1, 2), 1.5g of a catalyst (DBSA (dodecylbenzenesulfonic acid)), 1g of an initiator (azobisisobutylamidine hydrochloride), and performing high-speed shearing emulsification to obtain an emulsion; and (3) adjusting the temperature of the emulsion to 65 ℃, keeping the temperature at 75 ℃ for 3h, and adjusting the pH value of the emulsion to 7 to obtain the organic silicon fluorine-free waterproof soft finishing agent.
Example 2: an organosilicon fluorine-free waterproof soft finishing agent is prepared by the following steps:
500g of deionized water was put into a reaction vessel, and 100g of an organosilicon polymer (50 g of an alkylsiloxane, 50g of modified silicone oil), 18g of a surfactant (MES: DMSS: CAB-35=1 2 SO 4 ) 5g of initiator (azobisisobutylimidazoline hydrochloride), and carrying out high-speed shearing emulsification to obtain emulsion; and (3) adjusting the temperature of the emulsion to 70 ℃, keeping the temperature at 80 ℃ for 8h, and adjusting the pH value of the emulsion to 7 to obtain the organic silicon fluoride-free waterproof soft finishing agent.
Example 3: an organosilicon fluorine-free waterproof soft finishing agent is prepared by the following steps:
putting 700g of deionized water into a reaction kettle, sequentially putting 100g of an organic silicon polymer (60 g of alkyl siloxane and 40g of modified silicone oil), 40g of a surfactant (MES: DMSS: CAB-35=1, 2), 10g of a catalyst (HCl) and 5g of an initiator (azobisisobutylimidazoline hydrochloride) into the reaction kettle, and carrying out high-speed shearing emulsification to obtain an emulsion; and (3) adjusting the temperature of the emulsion to 75 ℃, keeping the temperature at 85 ℃ for 12h, and adjusting the pH value of the emulsion to 7 to obtain the organic silicon fluoride-free waterproof soft finishing agent.
The above finishes were then used to make blankets, as described in examples 4-6 below.
Example 4: an organic silicon fluorine-free waterproof soft terylene baschel blanket comprises the following finishing process:
the preparation method comprises the steps of diluting an organic silicon fluorine-free waterproof agent prepared in the embodiment 1 to 10g/L working solution, preparing a coating finishing solution with 10g of a cross-linking agent (pentaerythritol-tri (3-aziridinyl) propionate 3g and vinyl triethoxysilane 7 g), soaking a polyester basal raschel blanket subjected to plasma etching treatment and alkali decrement pretreatment in a soaking solution for 0.5h, carrying out two-soaking and two-rolling, wherein the padder pressure is 0.3MPa, then pre-baking at 100 ℃ for 5min, baking at 150 ℃ for 1min, taking out, and cooling to obtain the organic silicon fluorine-free waterproof soft finished polyester basal raschel blanket.
Example 5: an organic silicon fluorine-free waterproof soft terylene baschel blanket comprises the following finishing process:
the organic silicon fluorine-free waterproof agent prepared in the embodiment 2 is diluted to 30g/L of working solution, 20g of cross-linking agent (pentaerythritol-tri (3-aziridinyl) propionate 10g and vinyl triethoxysilane 10 g) is prepared into coating finishing solution, then the polyester base raschel blanket subjected to plasma etching treatment and alkali decrement pretreatment is put into the dipping solution to be soaked for 1h, the two-dipping and two-rolling are carried out, the padder pressure is 0.4MPa, then the polyester base raschel blanket is pre-baked at 110 ℃ for 8min and baked at 175 ℃ for 3min, and the polyester base raschel blanket is taken out and cooled to obtain the organic silicon fluorine-free waterproof soft finished polyester base raschel blanket.
Example 6: an organic silicon fluorine-free waterproof soft terylene baschel blanket comprises the following finishing process:
diluting the organic silicon fluorine-free waterproof agent prepared in the step 3 to 50g/L of working solution, preparing coating finishing solution by mixing with 30g of cross-linking agent (pentaerythritol-tri (3-aziridinyl) propionate 21g and vinyl triethoxysilane 9 g), then soaking the terylene raschel blanket subjected to plasma etching treatment and alkali decrement pretreatment in the soaking solution for 1h, carrying out two-soaking and two-rolling, wherein the padder pressure is 0.5MPa, then pre-baking at 120 ℃ for 10min and baking at 190 ℃ for 5min, taking out and cooling to obtain the organic silicon fluorine-free waterproof soft finished terylene raschel blanket.
Comparative example 1: unfinished polyester based raschel blanket:
the same polyester base raschel blanket purchased from the market is washed for 2 to 3 times, and then is pre-baked for 8min at 110 ℃ and baked for 4min at 150 ℃. Taking out and cooling to obtain the comparative example 1.
Comparative example 2: a preparation method of a commercially available organic silicon fluorine-free waterproof polyester Raschel blanket comprises the following steps:
a commercially available organic silicon fluorine-free waterproof agent is diluted to 50g/L working solution, a coating finishing solution is prepared by 30kg of a cross-linking agent (21 kg of pentaerythritol-tri (3-aziridinyl) propionate and 9kg of vinyl triethoxysilane), then a polyester-based raschel blanket is placed into a soaking solution to be soaked for 1h, two-dipping and two-rolling are carried out, the padder pressure is 0.5MPa, then the padding is pre-dried at 120 ℃ for 10min and baked at 170 ℃ for 5min, and the padding is taken out and cooled to obtain the commercially available organic silicon fluorine-free waterproof polyester raschel blanket.
The waterproof tests were carried out on the silicone fluorine-free waterproof polyester raschel blankets prepared in examples 4 to 6 and the polyester raschel blankets prepared in comparative examples 1 and 2, and the test methods and test results were as follows:
the method for testing the waterproofness of the polyester-based Raschel blanket comprises the following steps: and (3) carrying out waterproof performance test on the sample according to an AATCC-22 spraying experiment: the sample with constant temperature and pressure is arranged on a sample frame clamp, is arranged on a fixed base horizontally forming an angle of 45 degrees, 250ml of distilled water or deionized water (the temperature is 20 +/-2 ℃ or 27 +/-2 ℃) is quickly and stably injected into a funnel, and is uniformly and continuously sprayed towards the center of the sample within 24-30 seconds through a spray head specified with the center of the sample. The samples after the test were rated.
The samples were rated for water resistance according to the AATCC-22 rating scale.
100 (ISO 5) - - -there was no wetting of the sprayed surface nor beading.
90 (ISO 4) - - -the wetted surface was not wetted, but was stained with water droplets.
80 (ISO 3) -the sprayed surface is wetted only at the spraying point.
70 (ISO 2) - -the drenched surface was only partially wetted.
60 (ISO 1) - -total wetting of the drenched surface.
0- -the surface to be showered and the other surface are wetted completely.
The carpet water repellency performance results are shown in the following table:
table 1: test meter for water-proof property of blanket
| Numbering | Comparative example 1 | Comparative example 2 | Example 4 | Example 5 | Example 6 |
| Water resistance rating | ISO1 | ISO4 | ISO5 | ISO5 | ISO5 |
The flexibility tests of the silicone fluorine-free waterproof polyester raschel blankets prepared in examples 4-6 and the polyester raschel blankets prepared in comparative examples 1 and 2 were carried out, and the test methods and test results are as follows:
the method for testing the softness of the Raschel blanket comprises the following steps: the softness test was carried out according to ZBW04002-86 softness test run for comparative example 1,2 and example 4,5,6: two test specimens of approximately 25.4X 25.4mm (1X 1 in.) were cut, 10 pieces in length and width. The 6.4mm length of the upper end of the specimen was clamped into the test clip and the 6.4mm length of the lower end overlapped the pendulum pointer tongue. The selection of the pointer pendulum load and the offset position should make the bending rigidity force in the center of the lower dial as much as possible, press the swing button, the sample rod will swing from left to right or from right to left, respectively read the reading when the sample is separated from the pendulum pointer tongue piece dial, and process the reading.
The sample softness rating was according to ZBW04002-86 rating scale:
1- -very soft;
2- -softness;
3- -softer;
4- -hard;
5- -hard;
6- -very hard.
Specific results are shown in the following table.
TABLE 2 oil-proof performance test chart for blanket
| Numbering | Comparative example 1 | Comparative example 2 | Example 4 | Example 5 | Example 6 |
| Softness grade | 2 | 4 | 2 | 3 | 3 |
In addition, the silicone fluorine-free waterproof polyester raschel blankets prepared in examples 4 to 6 and the polyester raschel blankets prepared in comparative examples 1 and 2 were subjected to mechanical property detection, and the detection results are shown in table 3 below.
Table 3 testing table for mechanical property of blanket
For purposes of explanation, specific nomenclature is used in the above description to provide a thorough understanding of the described embodiments. It will be apparent, however, to one skilled in the art that these specific details are not required in order to practice the embodiments described above. Thus, the foregoing descriptions of specific embodiments described herein are presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the embodiments to the precise form disclosed. It will be apparent to those skilled in the art that certain modifications, combinations, and variations can be made in light of the above teachings.
Claims (5)
1. A finishing process of an organic silicon fluoride-free waterproof soft polyester based Raschel blanket is characterized in that: the method comprises the following steps:
(1) Preparing an organic silicon fluoride-free waterproof soft finishing agent:
firstly, putting deionized water into a reaction kettle, then sequentially putting an organic silicon polymer, a surfactant, a catalyst and an initiator into the reaction kettle according to a proportion, and carrying out shearing emulsification to obtain an emulsion;
adjusting the temperature of the emulsion to 65-75 ℃ and 75-85 ℃, preserving the heat for 1-12h, and adjusting the pH value of the emulsion to 7 to obtain the organic silicon fluorine-free waterproof soft finishing agent;
the raw materials of the organic silicon fluorine-free waterproof soft finishing agent comprise the following components in parts by weight:
30-50% of organic silicon polymer,
1 to 5 percent of surfactant,
0.1 to 5 percent of catalyst,
0.1 to 2.5 percent of initiator,
the balance of deionized water;
the organic silicon polymer comprises alkyl siloxane and modified silicone oil, and the weight ratio of the alkyl siloxane to the modified silicone oil is 4-6;
the modified silicone oil is one or a mixture of more of carboxyl silicone oil, amino silicone oil and epoxy modified silicone oil, the viscosity of the modified silicone oil is 200-1500 (Pa 8729s), and the number average molecular weight is 15000-30000;
(2) Pretreatment:
firstly, processing a polyester-based Raschel blanket by using air plasma, then cleaning and drying the blanket after alkali decrement pretreatment;
(3) Soft waterproof finishing:
firstly, diluting the finishing agent prepared in the step (1) and then preparing the diluted finishing agent and a cross-linking agent into coating finishing liquid;
then, putting the polyester-based Raschel blanket pretreated in the step (2) into the coating finishing liquid for soaking treatment, and carrying out two-soaking and two-rolling;
then, pre-baking at 100-120 ℃ for 5-10 min, baking at 150-190 ℃ for 1-5 min, taking out, and cooling to obtain the organic silicon fluorine-free waterproof soft-finished Raschel blanket;
the alkali solution in the alkali decrement treatment is obtained by mixing one of sodium hydroxide and potassium hydroxide with one of sodium bicarbonate, sodium carbonate, sodium phosphate and potassium carbonate in a mass ratio of 1;
the air plasma etching treatment process comprises the following steps: a polyester-based raschel blanket suspended in a closed processing space, supplying a gas carbon dioxide for plasma etching into the closed space, and setting the pressure in the closed space to 5-20 Pa; the treatment time is 1-3min.
2. The finishing process according to claim 1, characterized in that: the alkyl siloxane is one or a mixture of more of octamethylcyclotetrasiloxane (D4), trifluoropropylmethylcyclotrisiloxane (D3F), tetramethyltetravinylcyclotetrasiloxane (D4V), methyltriethoxysilane (MTES), methyltrimethoxysilane (MTMS), phenyltriethoxysilane (KH-651), vinyltrimethoxysilane (KH-171), 3-methacryloxypropyltriethoxysilane (KH-571), gamma-aminopropyltriethoxysilane (KH-550) and gamma- (2, 3 epoxypropoxy) propyltrimethoxysilane (KH-560).
3. The finishing process according to claim 1 or 2, characterized in that: the surfactant comprises MES (sodium fatty acid methyl ester sulfonate), DMSS (disodium coconut monoethanolamide sulfosuccinate) and CAB-35 (cocamidopropyl betaine), wherein the mass ratio of MES to DMSS to CAB-35 is 1-2.
4. The finishing process according to claim 1 or 2, characterized in that: the catalyst is one of DBSA (dodecyl benzene sulfonic acid), H2SO4 and HCl.
5. The finishing process according to claim 1, characterized in that: the cross-linking agent is pentaerythritol-tri (3-aziridinyl) propionate and vinyl triethoxysilane, and the mass ratio of the pentaerythritol-tri (3-aziridinyl) propionate to the vinyl triethoxysilane is 3-6.
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| CN102587147A (en) * | 2012-02-17 | 2012-07-18 | 福建凤竹纺织科技股份有限公司 | Production process of fluoride-free waterproof breathable knitted fabric |
| CN107653672A (en) * | 2017-10-13 | 2018-02-02 | 浙江真爱毯业科技有限公司 | A kind of silk gum modified dacron Rachael blanket |
| CN109914108A (en) * | 2019-03-14 | 2019-06-21 | 东华大学 | A kind of dacron free-floride water-repellent finishing method |
| CN110670364A (en) * | 2019-11-13 | 2020-01-10 | 福建华峰新材料有限公司 | Organic silicon fluorine-free waterproof agent, preparation method thereof and waterproof fabric |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102587147A (en) * | 2012-02-17 | 2012-07-18 | 福建凤竹纺织科技股份有限公司 | Production process of fluoride-free waterproof breathable knitted fabric |
| CN107653672A (en) * | 2017-10-13 | 2018-02-02 | 浙江真爱毯业科技有限公司 | A kind of silk gum modified dacron Rachael blanket |
| CN109914108A (en) * | 2019-03-14 | 2019-06-21 | 东华大学 | A kind of dacron free-floride water-repellent finishing method |
| CN110670364A (en) * | 2019-11-13 | 2020-01-10 | 福建华峰新材料有限公司 | Organic silicon fluorine-free waterproof agent, preparation method thereof and waterproof fabric |
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