CN108690184A - A method of producing big bright chip for chemical cycle method - Google Patents

A method of producing big bright chip for chemical cycle method Download PDF

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Publication number
CN108690184A
CN108690184A CN201710222858.6A CN201710222858A CN108690184A CN 108690184 A CN108690184 A CN 108690184A CN 201710222858 A CN201710222858 A CN 201710222858A CN 108690184 A CN108690184 A CN 108690184A
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CN
China
Prior art keywords
chemical cycle
producing big
big bright
aqueous solution
bright chip
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710222858.6A
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Chinese (zh)
Inventor
楼宝良
符学州
余新健
戴以明
Original Assignee
ZHEJIANG JIABAO NEW FIBER GROUP CO Ltd
ZHEJIANG JIABAO POLYESTER Co Ltd
Zhejiang Beauty New Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by ZHEJIANG JIABAO NEW FIBER GROUP CO Ltd, ZHEJIANG JIABAO POLYESTER Co Ltd, Zhejiang Beauty New Material Co Ltd filed Critical ZHEJIANG JIABAO NEW FIBER GROUP CO Ltd
Priority to CN201710222858.6A priority Critical patent/CN108690184A/en
Publication of CN108690184A publication Critical patent/CN108690184A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16Dicarboxylic acids and dihydroxy compounds
    • C08G63/18Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181Acids containing aromatic rings
    • C08G63/183Terephthalic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide

Abstract

The present invention relates to a kind of methods producing big bright chip for chemical cycle method, which is characterized in that the specific steps are:The catalyst of ethylene glycol EG and dimethyl terephthalate (DMT) DMT reaction needs are added in a kettle, brightener and stabilizer, temperature is in 150 DEG C of -280 DEG C of progress ester exchange reactions, reaction is completed to generate BHET, by-product is methanol, BHET is all sent into polymeric kettle and carries out polymerisation, and temperature controls between 260 DEG C -310 DEG C, vacuum pressure 50kpa-250kpa;PET is generated after about 4.5 hours polymerisations.The positive effect of the present invention is:Because adding brightener, it is high to be sliced transparent and brightness.

Description

A method of producing big bright chip for chemical cycle method
Technical field
The present invention relates to technical field of textile production, and specifically, be a kind of produced for chemical cycle method has light to cut greatly The method of piece.
Background technology
Polyester slice is often referred to the sheet that the polyester raw material that polymerization obtains is sized generally to about 4*5*2 millimeters or so Grain.The process route of production of polyester has direct esterification (PTA methods) and ester-interchange method (DMT methods).PTA methods have consumption of raw materials The low, advantages such as the reaction time is short, oneself becomes the main technique and one preferred technique route of polyester from the eighties.Large-scale production line It is continuous production processes, semicontinuous and batch production process is then suitble to medium and small a variety of process units.The purposes of polyester is now wrapped Include fiber, the fields such as all kinds of containers, packaging material, film, film, engineering plastics.
The coloration of polyester is an overall target, is not only influenced by the external world such as PTA, delustering agent and catalyst, together When also influenced by itself production process in production of polyester.Gather caused by the influence of either external coloration or inherent quality Ester coloration is turned to be yellow, and so that the coloration of fiber is turned to be yellow, be influenced the appearance of fiber, and especially degradation or metal catalyst ion are made At coloration turn to be yellow burnt hair, be easy to make spinning process medium viscosity drop to increase, cause the fluctuation of spinning.B values in coloration are anti- What is reflected is the blue yellowing of polyester slice, and b values are smaller, then polyester color is more biased to blue, more Gao Yuehuang.The reflection of L values is slice Gray scale, L values are bigger, then be sliced it is brighter, it is smaller then more grey.Titanium dioxide is added as delustering agent in polyester product, uses Amount determines according to the demand of user, and in general bright chip content is less than 0.12%, semi-dulling chips generally 0.12~ Between 0.5%, the said firm's content is between 0.28~0.3%.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind to have light to cut greatly for the production of chemical cycle method The method of piece.
The purpose of the present invention is achieved through the following technical solutions:
A method of big bright chip being produced for chemical cycle method, the specific steps are:
Be added the catalyst that ethylene glycol EG and dimethyl terephthalate (DMT) DMT reactions need in a kettle, brightener with And stabilizer, temperature are completed to generate BHET in 150 DEG C of -280 DEG C of progress ester exchange reactions, reaction, by-product is methanol, and BHET is complete Portion is sent into polymeric kettle and carries out polymerisation, and temperature controls between 260 DEG C -310 DEG C, vacuum pressure 50kpa-250kpa;By PET is generated after about 4.5 hours polymerisations.
The brightener is the particle of silica-doped titanium dioxide.
The preparation method of the brightener, the specific steps are:
The aqueous solution of sodium metasilicate is added in the aqueous solution of titanyl sulfate, pH value is adjusted to 5-8 with acid, is 50 in temperature Shi Jinhang is aged 3h, and separating mixture carries out washing drying, rises to 240 DEG C in air with the heating rate of 2 DEG C/min, stops Then 60min rises to 400 DEG C with the heating rate of 10 DEG C/min again under anaerobic or oxygen deprivation atmosphere, stop 60min to get two The particle of silica-doping titanium dioxide;Its technological merit is, by silica-doped titanium dioxide, using titanyl sulfate to exist Titanium dioxide is generated when pyrolytic, is improved titanium dioxide in the distributing homogeneity of silica surface, is improved titanium dioxide Photocatalysis, antibacterial effect.
The molar concentration of the aqueous solution of titanyl sulfate is 1mol/L;
The molar concentration of the aqueous solution of sodium metasilicate is 0.5mol/L;
The volume ratio of the aqueous solution of the aqueous solution sodium metasilicate of titanyl sulfate is 3:1
Technological process is:Raw material preparation -- -- -- -- wrap polymerisation filter ester exchange reaction by cooling and dicing -- storage -- Dress.
Compared with prior art, the positive effect of the present invention is:
Because adding brightener, it is high to be sliced transparent and brightness.
Specific implementation mode
A kind of specific implementation mode for the method producing big bright chip for chemical cycle method of the present invention presented below.
Embodiment 1
A method of big bright chip being produced for chemical cycle method, the specific steps are:
Be added the catalyst that ethylene glycol EG and dimethyl terephthalate (DMT) DMT reactions need in a kettle, brightener with And stabilizer, temperature are completed to generate BHET in 150 DEG C of -280 DEG C of progress ester exchange reactions, reaction, by-product is methanol, and BHET is complete Portion is sent into polymeric kettle and carries out polymerisation, and temperature controls between 260 DEG C -310 DEG C, vacuum pressure 50kpa-250kpa;By PET is generated after about 4.5 hours polymerisations.
Technological process is:Raw material preparation -- -- -- -- wrap polymerisation filter ester exchange reaction by cooling and dicing -- storage -- Dress.
The particle of the silica-doped titanium dioxide of the brightener.
The aqueous solution of sodium metasilicate is added in the aqueous solution of titanyl sulfate, pH value is adjusted to 5-8 with acid, is 50 in temperature Shi Jinhang is aged 3h, and separating mixture carries out washing drying, rises to 240 DEG C in air with the heating rate of 2 DEG C/min, stops Then 60min rises to 400 DEG C with the heating rate of 10 DEG C/min again under anaerobic or oxygen deprivation atmosphere, stop 60min to get two The particle of silica-doping titanium dioxide;
The molar concentration of the aqueous solution of titanyl sulfate is 1mol/L;
The molar concentration of the aqueous solution of sodium metasilicate is 0.5mol/L;
The volume ratio of the aqueous solution of the aqueous solution sodium metasilicate of titanyl sulfate is 3:1.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art Member, without departing from the inventive concept of the premise, can also make several improvements and modifications, these improvements and modifications also should be regarded as In protection scope of the present invention.

Claims (8)

1. a kind of method producing big bright chip for chemical cycle method, which is characterized in that the specific steps are:
It is added the catalyst that ethylene glycol EG and dimethyl terephthalate (DMT) DMT reactions need in a kettle, brightener and steady Determine agent, temperature is completed to generate BHET in 150 DEG C of -280 DEG C of progress ester exchange reactions, reaction, and by-product is methanol, and BHET is all sent Enter polymeric kettle and carry out polymerisation, temperature controls between 260 DEG C -310 DEG C, vacuum pressure 50kpa-250kpa;By about PET is generated after 4.5 hours polymerisations.
2. a kind of method producing big bright chip for chemical cycle method as described in claim 1, which is characterized in that raw material Proportioning is:
3. a kind of method producing big bright chip for chemical cycle method as described in claim 1, which is characterized in that technique Flow is:Raw material preparation -- -- -- -- pack polymerisation filter ester exchange reaction by cooling and dicing -- storage --.
4. a kind of method producing big bright chip for chemical cycle method as described in claim 1, which is characterized in that described Brightener be silica-doped titanium dioxide particle.
5. a kind of method producing big bright chip for chemical cycle method as described in claim 1, which is characterized in that described Brightener preparation method, the specific steps are:The aqueous solution of sodium metasilicate is added in the aqueous solution of titanyl sulfate, it will with acid PH value is adjusted to 5-8, carries out ageing 3h when temperature is 50, separating mixture carries out washing drying, in air with 2 DEG C/min Heating rate rise to 240 DEG C, 60min is stopped, then again with the heating rate liter of 10 DEG C/min under anaerobic or oxygen deprivation atmosphere To 400 DEG C, 60min is stopped to get the particle of silica-doped titanium dioxide.
6. a kind of method producing big bright chip for chemical cycle method as claimed in claim 5, which is characterized in that sulfuric acid The molar concentration of the aqueous solution of oxygen titanium is 1mol/L.
7. a kind of method producing big bright chip for chemical cycle method as claimed in claim 5, which is characterized in that silicic acid The molar concentration of the aqueous solution of sodium is 0.5mol/L.
8. a kind of method producing big bright chip for chemical cycle method as claimed in claim 5, which is characterized in that sulfuric acid The volume ratio of the aqueous solution of the aqueous solution sodium metasilicate of oxygen titanium is 3:1.
CN201710222858.6A 2017-04-07 2017-04-07 A method of producing big bright chip for chemical cycle method Pending CN108690184A (en)

Priority Applications (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110938198A (en) * 2019-11-20 2020-03-31 浙江佳人新材料有限公司 Production process of regenerated low-viscosity slices
CN113773477A (en) * 2021-09-08 2021-12-10 浙江佳人新材料有限公司 Method for preparing modified engineering polyester by using byproducts generated after chemical method cyclic regeneration of fiber vitamins

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1264852A2 (en) * 2001-06-07 2002-12-11 Montefibre S.p.A. Process for the preparation of polyester resins
CN1389490A (en) * 2002-07-05 2003-01-08 孙启明 Production process of polyethylene glycol terephthalate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1264852A2 (en) * 2001-06-07 2002-12-11 Montefibre S.p.A. Process for the preparation of polyester resins
CN1389490A (en) * 2002-07-05 2003-01-08 孙启明 Production process of polyethylene glycol terephthalate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李志林等: ""TiO2 /SiO2复合粉体的简易研磨法制备"", 《科学技术与工程》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110938198A (en) * 2019-11-20 2020-03-31 浙江佳人新材料有限公司 Production process of regenerated low-viscosity slices
CN113773477A (en) * 2021-09-08 2021-12-10 浙江佳人新材料有限公司 Method for preparing modified engineering polyester by using byproducts generated after chemical method cyclic regeneration of fiber vitamins
CN113773477B (en) * 2021-09-08 2023-02-17 浙江佳人新材料有限公司 Method for preparing modified engineering polyester by using byproducts generated after chemical method cyclic regeneration of fiber vitamins

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Effective date of registration: 20191126

Address after: 312071 building 7, No. 5, Paojiang Haitang Road, Shaoxing, Zhejiang Province

Applicant after: Zhejiang beauty New Material Co., Ltd.

Address before: 312071 Zhejiang city of Shaoxing Province on economic and Technological Development Zone Paojiang Road No. 5

Applicant before: Zhejiang beauty New Material Co., Ltd.

Applicant before: Zhejiang Jiabao New Fiber Group Co., Ltd.

Applicant before: ZHEJIANG JIABAO POLYESTER CO., LTD.

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Application publication date: 20181023

RJ01 Rejection of invention patent application after publication