CN105734974A - Benzophenone ultraviolet-proof finishing agent and preparation method thereof - Google Patents

Benzophenone ultraviolet-proof finishing agent and preparation method thereof Download PDF

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Publication number
CN105734974A
CN105734974A CN201610110950.9A CN201610110950A CN105734974A CN 105734974 A CN105734974 A CN 105734974A CN 201610110950 A CN201610110950 A CN 201610110950A CN 105734974 A CN105734974 A CN 105734974A
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parts
finishing agent
class anti
benzophenone class
ultraviolet finishing
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CN201610110950.9A
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Inventor
钱华
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SUZHOU FANGYOU NEW MATERIAL Co Ltd
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SUZHOU FANGYOU NEW MATERIAL Co Ltd
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Priority to CN201610110950.9A priority Critical patent/CN105734974A/en
Publication of CN105734974A publication Critical patent/CN105734974A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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 oxygen
    • D06M13/152Treating 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 oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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 oxygen
    • D06M13/165Ethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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 oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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
    • D06M13/325Amines
    • D06M13/335Amines having an amino group bound to a carbon atom of a six-membered aromatic ring
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • D06M15/09Cellulose ethers

Abstract

The invention discloses a benzophenone ultraviolet-proof finishing agent which comprises the following components in parts by weight: 10-20 parts of 2-amino-3',5-dichlorodibenzophenone, 12-18 parts of 3,5-diphenyl salicylaldehyde, 6-13 parts of diethyl phthalate, 3-9 parts of ethoxylated normal primary alcohol, 3-7 parts of hydroxymethyl cellulose, 1-5 parts of ammonium sulfate, 15-25 parts of polyvinyl alcohol, 3-8 parts of p-toluenesulfonic acid, 18-25 parts of ethylene glycol and 25-40 parts of deionized water. Clothes applied with the finishing agent have the excellent and lasting ultraviolet light absorbability and ultraviolet light intercepting and shielding effects, and have good absorption and transformation as well as reflection and scattering functions on ultraviolet light at the waveband of 320-400 nm.

Description

A kind of benzophenone class anti-ultraviolet finishing agent and preparation method thereof
Technical field
The invention belongs to finishing agent field, be specifically related to a kind of benzophenone class anti-ultraviolet finishing agent and preparation method thereof.
Background technology
The excessively exploitation of the earth is caused Earth'S atmosphere to be destroyed by people, and particularly ozone layer becomes dilute day by day Thin, amount of ultraviolet irradiation increases, and the disease thus caused also gets more and more.Some results of study show, the ultraviolet that excess is too strong Line irradiates particularly evident to the injury of human skin, and the lighter causes skin burn, dry, coarse etc., severe one initiation skin carcinoma etc. Disease.Nowadays, increasing people likes Our Nature, and embracing the Nature, outdoor travel and exploration also becomes a kind of new Popular and trend, they mostly use sunscreen cream etc. to carry out ultraviolet protection, but have the sunscreen cream of good sun-proof result also Anaphylaxis dermatosis can be caused, and existing clothes overcoat does not has good anti-ultraviolet function.
Summary of the invention
For above technical problem present in prior art, the present invention provide a kind of benzophenone class anti-ultraviolet finishing agent and Its preparation method, so that utilizing the medicated clothing of this finishing agent to have excellent durable UV absorbing properties and ultraviolet baffle plate Cover effect.
Technical scheme: a kind of benzophenone class anti-ultraviolet finishing agent, including the composition of following parts by weight: 2-amino-3', 5- Dichlorobenzophenone 10-20 part, 3,5-diphenyl salicylide 12-18 parts, ethyl phthalate 6-13 part, ethoxylated linear primary alconol 3- 9 parts, hydroxymethyl cellulose 3-7 part, ammonium sulfate 1-5 part, polyvinyl alcohol 15-25 part, p-methyl benzenesulfonic acid 3-8 part, ethylene glycol 18-25 Part, deionized water 25-40 part.
Preferably, described 2-amino-3', 5-dichlorobenzophenone 12-16 part, 3,5-diphenyl salicylide 14-17 parts, phthalandione Diethylester 8-11 part, ethoxylated linear primary alconol 5-8 part, hydroxymethyl cellulose 5-7 part, ammonium sulfate 2-4 part, polyvinyl alcohol 18- 22 parts, p-methyl benzenesulfonic acid 4-7 part, ethylene glycol 20-23 part, deionized water 30-35 part.
Preferably, described 2-amino-3', 5-dichlorobenzophenone 14 parts, 3,5-diphenyl salicylides 16 parts, ethyl phthalate 9 parts, ethoxylated linear primary alconol 7 parts, hydroxymethyl cellulose 6 parts, 3 parts of ammonium sulfate, polyvinyl alcohol 20 parts, p-methyl benzenesulfonic acid 5 parts, Ethylene glycol 22 parts, deionized water 33 parts.
The preparation method of a kind of benzophenone class anti-ultraviolet finishing agent, specifically includes following steps:
(1) by ethyl phthalate 6-13 part, ethoxylated linear primary alconol 3-9 part, hydroxymethyl cellulose 3-7 part and polyethylene Alcohol 15-25 part adds in 2-amino-3', 5-dichlorobenzophenone 10-20 part, and mix and blend heating-up temperature is to 60-75 DEG C, and insulation is anti- Answer 2-4h, obtain mixed liquor A;
(2) p-methyl benzenesulfonic acid 3-8 part and ethylene glycol 18-25 part are added 3, in 5-diphenyl salicylide 12-18 part, mixing Agitating heating temperature to 70-80 DEG C, insulation reaction 1.5-3h, obtain mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 25-40 part, rise High-temperature, to 40-50 DEG C, adds ammonium sulfate 1-5 part, standing and reacting 2-3.5h after dropping while stirring, and band reactant liquor cools down After i.e. can get described benzophenone class anti-ultraviolet finishing agent.
Preferably, described in step (1), temperature is 68 DEG C, insulation reaction 3h, and the speed of stirring is 300-400r/min.
Preferably, described in step (2), temperature is 75 DEG C, insulation reaction 2h, and the speed of stirring is 350-450r/min.
Preferably, described in step (3), temperature is 45 DEG C, and time for adding is 5-8min, standing and reacting 3h.
Beneficial effect: the preparation method of a kind of benzophenone class anti-ultraviolet finishing agent of the present invention, by add 2-amino- 3', 5-dichlorobenzophenone, 3, the raw material such as 5-diphenyl salicylide and ethyl phthalate, blended, stir, prepared by the technique such as heating Obtain benzophenone class anti-ultraviolet finishing agent;This preparation technology is simple, process is shorter, is suitable for large-scale production, applies the present invention Medicated clothing after finishing agent has excellent durable UV absorbing properties and ultraviolet blocking shield effectiveness, to 320~400nm ripples The ultraviolet of section has good sorption enhanced, reflection and scattering process.
Detailed description of the invention
Embodiment 1
(1) by ethyl phthalate 6 parts, ethoxylated linear primary alconol 3 parts, hydroxymethyl cellulose 3 parts and polyvinyl alcohol 15 parts Adding 2-amino-3', in 5-dichlorobenzophenone 10 parts, mix and blend heating-up temperature to 60 DEG C, the speed of stirring is 300r/min, Insulation reaction 2h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 3 parts and ethylene glycol 18 parts being added 3, in 5-diphenyl salicylide 12 parts, mix and blend heats Temperature is to 70 DEG C, and the speed of stirring is 350r/min, and insulation reaction 1.5h obtains mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 25 parts, raise Temperature, to 40 DEG C, adds 1 part of ammonium sulfate while stirring, and time for adding 5min, standing and reacting 2h after dropping, band reactant liquor is cold The most i.e. can get described benzophenone class anti-ultraviolet finishing agent.
Comparative example 1
(1) by ethoxylated linear primary alconol 3 parts, hydroxymethyl cellulose 3 parts and 15 parts of mix and blend heating temperature of polyvinyl alcohol Degree is to 60 DEG C, and the speed of stirring is 300r/min, and insulation reaction 2h obtains mixed liquor A;
(2) by p-methyl benzenesulfonic acid 3 parts and 18 parts of mix and blend heating-up temperatures of ethylene glycol to 70 DEG C, the speed of stirring is 350r/min, insulation reaction 1.5h, obtain mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 25 parts, raise Temperature, to 40 DEG C, adds 1 part of ammonium sulfate while stirring, and time for adding 5min, standing and reacting 2h after dropping, band reactant liquor is cold The most i.e. can get finishing agent.
Embodiment 2
(1) by ethyl phthalate 13 parts, ethoxylated linear primary alconol 9 parts, hydroxymethyl cellulose 7 parts and polyvinyl alcohol 25 parts Adding 2-amino-3', in 5-dichlorobenzophenone 20 parts, mix and blend heating-up temperature to 75 DEG C, the speed of stirring is 400r/min, Insulation reaction 4h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 8 parts and ethylene glycol 25 parts being added 3, in 5-diphenyl salicylide 18 parts, mix and blend heats Temperature is to 80 DEG C, and the speed of stirring is 450r/min, and insulation reaction 3h obtains mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 40 parts, raise Temperature, to 50 DEG C, adds 5 parts of ammonium sulfate, time for adding 8min, standing and reacting 3.5h after dropping, band reactant liquor while stirring Described benzophenone class anti-ultraviolet finishing agent is i.e. can get after cooling.
Comparative example 2
(1) by ethoxylated linear primary alconol 9 parts, hydroxymethyl cellulose 7 parts and 25 parts of mix and blend heating temperature of polyvinyl alcohol Degree is to 75 DEG C, and the speed of stirring is 400r/min, and insulation reaction 4h obtains mixed liquor A;
(2) by p-methyl benzenesulfonic acid 8 parts and 25 parts of mix and blend heating-up temperatures of ethylene glycol to 80 DEG C, the speed of stirring is 450r/min, insulation reaction 3h, obtain mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 40 parts, raise Temperature, to 50 DEG C, adds 5 parts of ammonium sulfate, time for adding 8min, standing and reacting 3.5h after dropping, band reactant liquor while stirring Finishing agent is i.e. can get after cooling.
Embodiment 3
(1) by ethyl phthalate 8 parts, ethoxylated linear primary alconol 5 parts, hydroxymethyl cellulose 5 parts and polyvinyl alcohol 18 parts Adding 2-amino-3', in 5-dichlorobenzophenone 12 parts, mix and blend heating-up temperature to 60 DEG C, the speed of stirring is 300r/min, Insulation reaction 2h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 4 parts and ethylene glycol 20 parts being added 3, in 5-diphenyl salicylide 14 parts, mix and blend heats Temperature is to 70 DEG C, and the speed of stirring is 350r/min, and insulation reaction 1.5h obtains mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 30 parts, raise Temperature, to 40 DEG C, adds 2 parts of ammonium sulfate while stirring, and time for adding 5min, standing and reacting 2h after dropping, band reactant liquor is cold The most i.e. can get described benzophenone class anti-ultraviolet finishing agent.
Embodiment 4
(1) by ethyl phthalate 11 parts, ethoxylated linear primary alconol 8 parts, hydroxymethyl cellulose 7 parts and polyvinyl alcohol 22 parts Adding 2-amino-3', in 5-dichlorobenzophenone 16 parts, mix and blend heating-up temperature to 75 DEG C, the speed of stirring is 400r/min, Insulation reaction 4h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 7 parts and ethylene glycol 23 parts being added 3, in 5-diphenyl salicylide 17 parts, mix and blend heats Temperature is to 80 DEG C, and the speed of stirring is 450r/min, and insulation reaction 3h obtains mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 35 parts, raise Temperature, to 50 DEG C, adds 4 parts of ammonium sulfate, time for adding 8min, standing and reacting 3.5h after dropping, band reactant liquor while stirring Described benzophenone class anti-ultraviolet finishing agent is i.e. can get after cooling.
Embodiment 5
(1) by ethyl phthalate 14 parts, ethoxylated linear primary alconol 7 parts, hydroxymethyl cellulose 6 parts and polyvinyl alcohol 20 parts Adding 2-amino-3', in 5-dichlorobenzophenone 14 parts, mix and blend heating-up temperature to 68 DEG C, the speed of stirring is 350r/min, Insulation reaction 3h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 5 parts and ethylene glycol 23 parts being added 3, in 5-diphenyl salicylide 16 parts, mix and blend heats Temperature is to 75 DEG C, and the speed of stirring is 400r/min, and insulation reaction 2h obtains mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 33 parts, raise Temperature, to 45 DEG C, adds 3 parts of ammonium sulfate while stirring, and time for adding 6min, standing and reacting 3h after dropping, band reactant liquor is cold The most i.e. can get described benzophenone class anti-ultraviolet finishing agent.
By the finishing agent obtained by each embodiment and comparative example, it is applied in textile clothes, tests treated weaving clothing The preventing ultraviolet effect of thing, result is as follows:
Experiment UPF UV-ray
Embodiment 1 29 5
Comparative example 1 5 25
Embodiment 2 30 3
Comparative example 2 8 20
Embodiment 3 35 2.5
Embodiment 4 45 2.0
Embodiment 5 50 1.5

Claims (7)

1. a benzophenone class anti-ultraviolet finishing agent, it is characterised in that include the composition of following parts by weight: 2-amino-3', 5- Dichlorobenzophenone 10-20 part, 3,5-diphenyl salicylide 12-18 parts, ethyl phthalate 6-13 part, ethoxylated linear primary alconol 3- 9 parts, hydroxymethyl cellulose 3-7 part, ammonium sulfate 1-5 part, polyvinyl alcohol 15-25 part, p-methyl benzenesulfonic acid 3-8 part, ethylene glycol 18-25 Part, deionized water 25-40 part.
A kind of benzophenone class anti-ultraviolet finishing agent the most according to claim 1, it is characterised in that described 2-amino-3', 5- Dichlorobenzophenone 12-16 part, 3,5-diphenyl salicylide 14-17 parts, ethyl phthalate 8-11 part, ethoxylated linear primary alconol 5- 8 parts, hydroxymethyl cellulose 5-7 part, ammonium sulfate 2-4 part, polyvinyl alcohol 18-22 part, p-methyl benzenesulfonic acid 4-7 part, ethylene glycol 20-23 Part, deionized water 30-35 part.
A kind of benzophenone class anti-ultraviolet finishing agent the most according to claim 2, it is characterised in that described 2-amino-3', 5- Dichlorobenzophenone 14 parts, 3,5-diphenyl salicylides 16 parts, ethyl phthalate 9 parts, ethoxylated linear primary alconol 7 parts, methylol Cellulose 6 parts, 3 parts of ammonium sulfate, polyvinyl alcohol 20 parts, p-methyl benzenesulfonic acid 5 parts, ethylene glycol 22 parts, deionized water 33 parts.
4. the preparation method of a benzophenone class anti-ultraviolet finishing agent, it is characterised in that specifically include following steps:
(1) by ethyl phthalate 6-13 part, ethoxylated linear primary alconol 3-9 part, hydroxymethyl cellulose 3-7 part and polyvinyl alcohol 15-25 part adds in 2-amino-3', 5-dichlorobenzophenone 10-20 part, mix and blend heating-up temperature to 60-75 DEG C, insulation reaction 2-4h, obtains mixed liquor A;
(2) p-methyl benzenesulfonic acid 3-8 part and ethylene glycol 18-25 part are added 3, in 5-diphenyl salicylide 12-18 part, mix and blend Heating-up temperature to 70-80 DEG C, insulation reaction 1.5-3h, obtain mixed liquid B;
(3) mixed liquid B described in mixed liquor A described in step (1) and step (2) is added deionized water 25-40 part, rise high temperature Degree, to 40-50 DEG C, adds ammonium sulfate 1-5 part, standing and reacting 2-3.5h after dropping while stirring, after the cooling of band reactant liquor is Available described benzophenone class anti-ultraviolet finishing agent.
The preparation method of a kind of benzophenone class anti-ultraviolet finishing agent the most according to claim 4, it is characterised in that step (1) temperature described in is 68 DEG C, insulation reaction 3h, and the speed of stirring is 300-400r/min.
The preparation method of a kind of benzophenone class anti-ultraviolet finishing agent the most according to claim 4, it is characterised in that step (2) temperature described in is 75 DEG C, insulation reaction 2h, and the speed of stirring is 350-450r/min.
The preparation method of a kind of benzophenone class anti-ultraviolet finishing agent the most according to claim 4, it is characterised in that step (3) temperature described in is 45 DEG C, and time for adding is 5-8min, standing and reacting 3h.
CN201610110950.9A 2016-02-29 2016-02-29 Benzophenone ultraviolet-proof finishing agent and preparation method thereof Pending CN105734974A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107740273A (en) * 2017-09-30 2018-02-27 江苏新瑞贝科技股份有限公司 A kind of anti-ultraviolet finishing agent and preparation method thereof

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CN104805693A (en) * 2015-05-12 2015-07-29 湖州厉华妤婕联合纺织有限公司 Novel ultraviolet-proof finishing agent composition for cotton fabric
CN104894855A (en) * 2015-06-15 2015-09-09 湖州厉华妤婕联合纺织有限公司 Novel ultraviolet-proof finishing agent for textile

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CN104805693A (en) * 2015-05-12 2015-07-29 湖州厉华妤婕联合纺织有限公司 Novel ultraviolet-proof finishing agent composition for cotton fabric
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CN107740273A (en) * 2017-09-30 2018-02-27 江苏新瑞贝科技股份有限公司 A kind of anti-ultraviolet finishing agent and preparation method thereof

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Application publication date: 20160706