CN103540108B - A kind of manufacture craft of crystallization nanometer PET - Google Patents
A kind of manufacture craft of crystallization nanometer PET Download PDFInfo
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- CN103540108B CN103540108B CN201310430786.6A CN201310430786A CN103540108B CN 103540108 B CN103540108 B CN 103540108B CN 201310430786 A CN201310430786 A CN 201310430786A CN 103540108 B CN103540108 B CN 103540108B
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Abstract
The invention discloses a kind of manufacture craft of crystallization nanometer PET, its processing step is: (1) raw material prepares; (2) blended; Mixed with ethylene glycol (EG) by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, adds CaCO3 organic filler in described mixed solution, and the mass content of described weighting agent is 3% ~ 5%; (3) permutoid reaction; (4) polycondensation; (5) enhancing modified; (6) Crystallization Separation, by to after a series of process of raw material, PET rubber is made not only in wide temperature range, to have excellent physical and mechanical properties, electrical insulating property is excellent, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, has the features such as stronger shock resistance.
Description
Technical field
The manufacture craft of the plastic material that the present invention relates to, particularly relates to a kind of manufacture craft of crystallization nanometer PET.
Background technology
At present, plastics have been widely used in the fields such as construction industry, wrapping material, family daily necessity and automobile.Plastics because of its widely purposes and good use properties and and iron and steel, timber, one of cement four large base mateirals constituting modern industry, PET is polyethylene terephthalate plastics, be commonly called as polyester resin, it is the polycondensate of terephthalic acid and ethylene glycol, thermoplastic polyester is referred to as together with PBT, or saturated polyester, PET molecular structure high degree of symmetry, there is certain crystalline orientation ability, so there is higher film-forming properties and become second nature, PET has good optical property and weathering resistance, amorphous PET has good optical transparence, PET has bottle that excellent abrasion performance frictional property and dimensional stability and electrical insulating property PET make to have intensity large in addition, the transparency is good, nontoxic, impermeable, quality is light, high thus the receiving of production efficiency is applied widely, but PET plastics crystallization velocity is slow, shock resistance is poor, not easily process.
Summary of the invention
For overcoming the deficiency in prior art, the object of the invention is to provide a kind of manufacture craft of crystallization nanometer PET.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A manufacture craft for crystallization nanometer PET, its processing step is as follows:
(1) raw material prepares; Under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing Zinc compounds is catalyzer, crude terephthalic acid is made high purity terephthalic acid (PTA), and getting its purity is 98%;
(2) blended; Mixed with ethylene glycol (EG) by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, adds CaCO in described mixed solution
3inorganic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) esterification; Catalyzer is added in the mixture of step (2), under the effect of catalyzer, terephthalic acid and ethylene glycol generation esterification, described catalyzer is zinc, cobalt, the acetate of manganese and the mixture of antimonous oxide, and described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation; The reaction product of step (3) is imported polycondensation vessel, and controlling temperature of reaction is 270 DEG C ~ 280 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) enhancing modified; In polycondensation vessel, add plastics toughener, nano flame retardant mixture, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant mixture is:
1. silicone hydroxyl phosphatic rock, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of dimethyl sulfoxide (DMSO) (DMSO) and 50 parts of methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive dimethyl sulfoxide (DMSO) (DMSO) of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying oven, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant mixture;
2. by 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water mixing, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition.To filter, and with distilling washing 3 times, 80 DEG C of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
3. above-mentioned 1 part of twice-modified flame-retardant compounds is disperseed 40min at 600W power ultrasonic, be heated to 90 DEG C with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain nano flame retardant mixture;
(6) Crystallization Separation; Crystallization operation is carried out to the mixture after step (4), temperature controlled at 200 DEG C ~ 210 DEG C, drop into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET after crystallization.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET, wherein, in described step (3), described esterification is carried out under pH is the acidic conditions of 5 ~ 6.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET, wherein, in described step (4), described polyester migrates out polycondensation vessel gradually along with reaction.
The manufacture craft of above-mentioned a kind of crystallization nanometer PET, wherein, in described step (6), described PET obtains the finished product through washing drying.
Beneficial effect: make raw material through preparing, blended, esterification, polycondensation, enhancing modified, Crystallization Separation six steps, PET rubber is made not only in wide temperature range, to have excellent physical and mechanical properties, electrical insulating property is excellent, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the features such as stronger shock resistance, the terephthalic acid of high-purity during raw material prepares, guarantee the high purity of plastics product, enhance productivity, organic filler is added in Blending Processes, plastics are made to be easy to processing, in esterification, catalyzer chooses, greatly improve reaction plastics, the control of temperature of reaction is better ensure that the physical and mechanical properties of the excellence of plastics and the stable of size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener added makes plastics possess very strong shock resistance, the crystallization promoter used in Crystallization Separation operation, make the crystallization velocity of plastics fast, raise the efficiency, be convenient to collect, acid condition has katalysis to esterification, product is shifted out reactor simultaneously, more accelerate the generation of plastics.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, and such benefit is: increase reactive behavior point, improves modified effect; Can steam again except the moisture in system while modification, dry and modification is carried out simultaneously, improves working efficiency; There is a large amount of physics and chemistry planar water in self micropore such as nano silicone hydroxyapatite, Attapulgite, polynite, kaolin, at high temperature produce water vapor, block oxygen, absorb heat, reach multiple fire-retardant effect; Powerful absorption property effectively can improve the synergy of several fire retardant, stops and is raised by fire retardant matter temperature, improve flame retarding efficiency; The aboundresources such as silicone hydroxyl phosphatic rock, Attapulgite, polynite, kaolin, greatly reduces the industrial cost of fire retardant, also for the Application and Development of attapulgite provides a new way; The present invention adopt solution method ultrasonic wave disperse and mechanical high-speed agitator stir, make fire retardant separately component reach nano-scale dispersion in the solution, effectively prevent the natural oxidation to matrix material, thus make matrix material have better mechanical property.The oxygen index of matrix material is 41.
Embodiment
The technique means realized for making the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with embodiment, setting forth the present invention further.
Embodiment 1:
The manufacture craft of a kind of crystallization nanometer PET of the present embodiment, its processing step is as follows:
(1) raw material prepares; Under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing Zinc compounds is catalyzer, crude terephthalic acid is made high purity terephthalic acid (PTA), and getting its purity is 98%;
(2) blended; Mixed with ethylene glycol (EG) by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, adds CaCO in described mixed solution
3inorganic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) esterification; Catalyzer is added in the mixture of step (2), under the effect of catalyzer, terephthalic acid and ethylene glycol generation esterification, described catalyzer is zinc, cobalt, the acetate of manganese and the mixture of antimonous oxide, and described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation; The reaction product of step (3) is imported polycondensation vessel, and controlling temperature of reaction is 270 DEG C ~ 280 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) enhancing modified; In polycondensation vessel, add plastics toughener, nano flame retardant mixture, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant mixture is:
1. silicone hydroxyl phosphatic rock, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of dimethyl sulfoxide (DMSO) (DMSO) and 50 parts of methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive dimethyl sulfoxide (DMSO) (DMSO) of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying oven, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant mixture;
2. by 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water mixing, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition.To filter, and with distilling washing 3 times, 80 DEG C of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
3. above-mentioned 1 part of twice-modified flame-retardant compounds is disperseed 40min at 600W power ultrasonic, be heated to 90 DEG C with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain nano flame retardant mixture;
(6) Crystallization Separation; Crystallization operation is carried out to the mixture after step (4), temperature controlled at 200 DEG C ~ 210 DEG C, drop into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET after crystallization.
Wherein, in described step (3), described esterification is carried out under pH is the acidic conditions of 5 ~ 6,
And in described step (6), described PET obtains the finished product through washing drying.
Embodiment 2: all the other are identical with described embodiment 1, and difference is, the terephthalic acid purity prepared in step (1) is medium, in the present embodiment, advantage of lower cost, but the speed of reaction making plastics is slow, and efficiency is low, and plastics physicals reduces.
Embodiment 3: all the other are identical with described embodiment 1, and difference is, changes crystallization promoter in step (6): changing Sodium Benzoate is organic montmorillonoid, and in this enforcement, corresponding temperature of reaction increases, and crystallization effect is poorer than embodiment 1.
Known in practical application, make raw material through preparing, blended, esterification, polycondensation, enhancing modified, Crystallization Separation six steps, PET rubber is made not only in wide temperature range, to have excellent physical and mechanical properties, electrical insulating property is excellent, creep resistance, resistance to fatigue, rub resistance, good stability of the dimension, and crystallization rate is fast, forming process is easy, there is the features such as stronger shock resistance, the terephthalic acid of high-purity during raw material prepares, guarantee the high purity of plastics product, enhance productivity, organic filler is added in Blending Processes, plastics are made to be easy to processing, in esterification, catalyzer chooses, greatly improve reaction plastics, the control of temperature of reaction is better ensure that the physical and mechanical properties of the excellence of plastics and the stable of size, under the condition of high vacuum and strong mixing, reaction generates the polyester of high molecular, the plastics toughener added makes plastics possess very strong shock resistance, the crystallization promoter used in Crystallization Separation operation, make the crystallization velocity of plastics fast, raise the efficiency, be convenient to collect, acid condition has katalysis to esterification, product is shifted out reactor simultaneously, more accelerate the generation of plastics.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, has a extensive future; The present invention carries out twice-modified, and such benefit is: increase reactive behavior point, improves modified effect; Can steam again except the moisture in system while modification, dry and modification is carried out simultaneously, improves working efficiency; There is a large amount of physics and chemistry planar water in self micropore such as nano silicone hydroxyapatite, Attapulgite, polynite, kaolin, at high temperature produce water vapor, block oxygen, absorb heat, reach multiple fire-retardant effect; Powerful absorption property effectively can improve the synergy of several fire retardant, stops and is raised by fire retardant matter temperature, improve flame retarding efficiency; The aboundresources such as silicone hydroxyl phosphatic rock, Attapulgite, polynite, kaolin, greatly reduces the industrial cost of fire retardant, also for the Application and Development of attapulgite provides a new way; The present invention adopt solution method ultrasonic wave disperse and mechanical high-speed agitator stir, make fire retardant separately component reach nano-scale dispersion in the solution, effectively prevent the natural oxidation to matrix material, thus make matrix material have better mechanical property.The oxygen index of matrix material is 41.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (3)
1. a manufacture craft for crystallization nanometer PET, is characterized in that, its processing step is as follows:
(1) raw material prepares: under temperature of reaction 250 ~ 300 DEG C and reaction pressure 2 ~ 2.5MPa condition, employing Zinc compounds is catalyzer, and crude terephthalic acid is made high purity terephthalic acid, and getting its purity is 98%;
(2) blended: to be mixed with ethylene glycol (EG) by terephthalic acid made for step (1), the mass ratio of described terephthalic acid and ethylene glycol (EG) is 1:1.5 ~ 2, adds CaCO in described mixed solution
3inorganic filler, the mass content of described weighting agent is 3% ~ 5%;
(3) esterification: add catalyzer in the mixture of step (2), under the effect of catalyzer, terephthalic acid and ethylene glycol generation esterification, described catalyzer is zinc, cobalt, the acetate of manganese and the mixture of antimonous oxide, and described catalyst levels is 0.01% ~ 0.05% of terephthalic acid quality;
(4) polycondensation: the reaction product of step (3) is imported polycondensation vessel, controlling temperature of reaction is 270 DEG C ~ 280 DEG C, carries out under high vacuum and strong mixing, obtains the polyester of high molecular;
(5) enhancing modified: add plastics toughener, nano flame retardant mixture in polycondensation vessel, stir simultaneously, described plastics toughener is DH-4 toughener, and its consumption is 6 ~ 8%; Described nano flame retardant mixture is 10%-15%,
The preparation method of described nano flame retardant mixture is:
1. silicone hydroxyl phosphatic rock, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of dimethyl sulfoxide (DMSO) (DMSO) and 50 parts of methyl alcohol, stir 60 hours in 65 DEG C, filter, and wash the excessive dimethyl sulfoxide (DMSO) (DMSO) of 3 removings with the hot ethanol of 60 DEG C of temperature, put into vacuum drying oven, 60 DEG C of temperature dryings 24 hours, grinding is sieved, and obtains a modified flame-retardant mixture;
2. by 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water mixing, more than 10 hours are stirred in temperature 50 C, in temperature 30 DEG C, first disperse 2.5 hours under ultrasonic electric power 350W condition, and then disperse 3 hours under ultrasonic electric power 250W condition
,to filter, and with distilling washing 3 times, 80 DEG C of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified flame-retardant compounds;
3. above-mentioned 1 part of twice-modified flame-retardant compounds is disperseed 40min at 600W power ultrasonic, be heated to 90 DEG C with constant temperature heating device, and stir with mechanical stirrer, 1200r/min stirs 60 minutes; Obtain nano flame retardant mixture;
(6) crystallization: crystallization is carried out to the mixture after step (4), temperature controlled at 200 DEG C ~ 210 DEG C, drop into crystallization promoter, described crystallization promoter is Sodium Benzoate, described Sodium Benzoate consumption is 0.9 ~ 1.5% of terephthalic acid quality, obtains PET after crystallization.
2. the manufacture craft of crystallization nanometer PET according to claim 1, is characterized in that, in described step (3), described esterification is carried out under pH is the acidic conditions of 5 ~ 6.
3. the manufacture craft of crystallization nanometer PET according to claim 1, is characterized in that, in described step (6), described PET obtains the finished product through washing drying.
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| CN104513464A (en) * | 2014-12-31 | 2015-04-15 | 广西大学 | Production process for PET plastic |
| CN104861185A (en) * | 2015-04-28 | 2015-08-26 | 安徽美翔塑业有限公司 | Thin film production process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030118817A1 (en) * | 2000-02-19 | 2003-06-26 | Ursula Murschall | Sealable, flame-resistant, co-extruded, biaxially oriented foil that is mat on one side and a method for producing and using same |
| CN101402722A (en) * | 2008-11-26 | 2009-04-08 | 吉林大学 | Method for preparing nano-calcium carbonate/polyester composite material |
| CN102002141A (en) * | 2010-11-19 | 2011-04-06 | 安徽大学 | Preparation method of polyurethane-nano kaolin composite material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030118817A1 (en) * | 2000-02-19 | 2003-06-26 | Ursula Murschall | Sealable, flame-resistant, co-extruded, biaxially oriented foil that is mat on one side and a method for producing and using same |
| CN101402722A (en) * | 2008-11-26 | 2009-04-08 | 吉林大学 | Method for preparing nano-calcium carbonate/polyester composite material |
| CN102002141A (en) * | 2010-11-19 | 2011-04-06 | 安徽大学 | Preparation method of polyurethane-nano kaolin composite material |
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