CN103741256B - A kind of preparation method of krill protein renaturation cellulose fibre - Google Patents
A kind of preparation method of krill protein renaturation cellulose fibre Download PDFInfo
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Abstract
The present invention relates to chemical fibre material field, disclose a kind of preparation method of krill protein renaturation cellulose fibre, comprise the following steps: Making viscose solution, for subsequent use; Preparation precrosslink krill protein solution: add sodium hydroxide solution, krill albumen and sulfomethylated lignin acid amide successively, stir 4-6 hour at 50-70 DEG C, be cooled to 35-45 DEG C of insulation and filter, gained filtrate is krill protein solution; In krill protein solution, add crosslinking agent, at 35-45 DEG C of insulation reaction 0.4 ~ 0.6h, prepare precrosslink krill protein solution; By spinning after viscose solution, precrosslink krill protein solution, crosslinking agent mixing.The fiber that the present invention obtains has good brute force, ensure that the brute force of fiber, improves feel and the gloss of fiber simultaneously, can be used as the raw material of textile industry.
Description
Technical field
The present invention relates to chemical fibre material field, particularly a kind of preparation method of krill protein renaturation cellulose fibre.
Background technology
Krill, as the maximum single living resources of Southern Oceans, is an important monoid in marine zooplankton, supports the population of the huge high-rise predator such as penguin, sea dog, cetacean.Except as except the key organism in biosystem, also because of huge biomass and potential fishery resources, be day by day subject to the attention of people.
In krill the AAS AAS (except threonine and valine) of essential amino acid all close to or be greater than 1; Chemical score CS (except threonine, valine and tryptophan) is all greater than 0.5, and this shows that krill muscle essential amino acid ratio of components comparatively balances, and rich content.But the content of lysine is very high in krill muscle, and lysine wretched insufficiency in cereal (vegetable protein), krill then can make up this shortcoming.Amino acid whose of krill/virtue value is 2.14, close to the level of normal person.High, low arylmethyl amino acid and mixture have hepatoprotective effect.
Because krill dietary protein origin is wide, and wherein higher to human body beneficiating ingredient, therefore the possibility of its spinning is studied by a lot of producer.But because viscose glue stoste is at about 20 DEG C, its spinnability and stability is better and krill albumen can form gel under the condition of about 20 DEG C, be difficult to viscose glue stoste compatible very well, and rheological characteristic and the viscosity of viscose glue stoste can be changed, the blended liquid spinnability of krill albumen/viscose glue stoste is finally caused to be deteriorated, and it is large to cause plug-hole to make to spin the change of front pressure, makes spinning have very large difficulty, the krill azelon being used as textile process at present does not also have to be seen.
China Patent No. 201210457178.X discloses a kind of preparation method of synthetic wig fiber, and the method for raw material, prepares artificial hair by co-blended spinning with krill shrimp albumen and sodium alginate.But carry out blended with krill albumen and sodium alginate soln in this patent, its obtained fiber strength is lower, is difficult to the raw material of industry as textile process.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of krill protein renaturation cellulose fibre, viscose glue wet processing is adopted in this manufacture method, take cellulose as carrier, by krill albumen graft crosslinking on fiber, by controlling krill protein concentration, method from the time and mixing that are mixed into spinning, take into account the dissolubility of rayon spinning liquid spinnability and krill albumen, solve blended liquid spinnability and consistency problem.The fiber produced has good brute force, can for weaving.
To achieve these goals, the technical solution used in the present invention is:
A preparation method for krill protein renaturation cellulose fibre, comprises the following steps;
Step (1), Making viscose solution, for subsequent use;
Step (2), preparation precrosslink krill protein solution: add sodium hydroxide solution, krill albumen and sulfomethylated lignin acid amide in a reservoir successively, at 50-70 DEG C, stir 4-6 hour, be cooled to 35-45 DEG C of insulation and filter, gained filtrate is krill protein solution; In krill protein solution, add crosslinking agent, at 35-45 DEG C of insulation reaction 0.4-0.6h, prepare precrosslink krill protein solution; The weight of the krill albumen added is the 5-20% of sodium hydroxide solution weight, and the weight that sulfomethylated lignin acid amide adds is the 0.3-1% of krill protein by weight, and the weight that crosslinking agent adds is the 1-2% of krill protein by weight;
Step (3), by viscose solution and, precrosslink krill protein solution, crosslinking agent mixing after spinning, dosage of crosslinking agent is 1 ~ 12% of the fine mass content of first in viscose solution, and in described precrosslink krill protein solution, the weight of krill albumen is 1 ~ 8% of the fine weight of first in rayon spinning stoste.
In step (2), add crosslinking agent carry out precrosslink, object is first cross-linked between protein molecular, krill albumen in the basic conditions, intermolecular active force is weakened, partially protein can be hydrolyzed into polypeptide, is even hydrolyzed into less molecule (amino acid), now in order to improve the active force between protein, by crosslinking agent, polypeptide, amino acid equimolecular and protein are carried out certain being cross-linked, thus improve the utilization of albumen.If the consumption of crosslinking agent very little, then act on not obvious; Consumption is too large, can be excessively crosslinked, thus filters rear road and spinning fibre forming property generation considerable influence.
In step (2), add dispersant is to be disperseed uniformly in the solution by protein macromolecule.If dispersant addition is comparatively large, be unfavorable for the deaeration of rear road spinning solution.Addition is too little, then do not have the effect of emulsion dispersion.
It is then to improve krill albumen retention rate in the fibre that step (3) adds crosslinking agent, makes krill albumen and processbearing astrocyte covalent bond, is cross-linked by first fibre in krill albumen and viscose.
As preferably, the mass fraction of step (2) sodium hydroxide solution is 3-10%.
As preferably, crosslinking agent is one or more in glutaraldehyde, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
As preferably, the method for dynamically mixing and static mixing during spinning, is adopted to mix.
As preferably, the whole process being mixed into spinning completed within 10 minutes.
beneficial effect
1, because krill albumen can form gel under the condition of about 20 DEG C, be difficult to viscose glue stoste compatible very well, and rheological characteristic and the viscosity of viscose glue stoste can be changed, finally cause the blended liquid spinnability of krill albumen/viscose glue stoste to be deteriorated, and it is large to cause plug-hole to make to spin the change of front pressure, cannot spinning.The present invention, by controlling krill protein concentration, method from the time and mixing that are mixed into spinning, takes into account the dissolubility of rayon spinning liquid spinnability and krill albumen, effectively can solve the problem that krill protein liquid can not be compatible very well with rayon spinning stoste.Fiber has good brute force, ensure that the brute force of fiber, improves feel and the gloss of fiber simultaneously, can be used as the raw material of textile industry.
The control of krill protein concentration: (1) the present invention controls the concentration of krill albumen by preferred dispersant, dispersant used has alkali resistance and can well be disperseed by protein emulsifying in the basic conditions.(2) when krill albumen falls at temperature, can condense, dispersant has the effect that can prevent from condensing.
Mixing and spinning: (1) krill albumen drops to less than 28 DEG C at temperature to start to condense, and along with the prolongation of time, coacervation is obvious, in order to alleviate the generation of this situation, in preceding working procedure, just adds dispersant.(2) can there is gelation along with the rising of temperature in rayon spinning liquid, when temperature is more than 32 DEG C, and less standby spinnability in spinning solution 1h.(3) in order to take into account both performances, simultaneously can also good mixed dissolution, do not change respective characteristic.Optimize: first above-mentioned krill protein solution is cooled to 28 DEG C-30 DEG C, insulation deaeration; By spinning front injection measurement pump, be injected into by a certain percentage in the viscose glue of deaeration completely, blended viscose fully mixes respectively through dynamic mixer and static mixer, finally sends into spinning, and whole process required time is shorter.
2, the krill albumen selected of the present invention, essential amino acid ratio of components comparatively balances, and rich content, the content of lysine is very high, and this is that in vegetable protein, lysine can not be compared.Meanwhile, amino acid whose of krill/virtue value is 2.14, close to the level of normal person, and high, low arylmethyl amino acid and mixture also have hepatoprotective effect.It is for common artificial beef plant is compared in fiber preparation, and animal protein more easily acts on human skin, more excellent to the skin-friendly of human body skin.
Detailed description of the invention
To contribute to understanding the present invention by following practical operation and embodiment, but not limit content of the present invention.
embodiment 1
The preparation of viscose solution: (Cotton Pulp is also known as refining cotton pulp for the Cotton Pulp of the fine mass content 93.5% of the employing degree of polymerization 500, first, take cotton linter as raw material, a kind of high purity cellulose through alkaline cooking, rinsing are refined), successively through dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, the operation such as deaeration prepare spinning viscose solution.Fine mass content 8.9%, the NaOH mass content 5.5% of obtained first, viscosity (falling ball method: the time that 2mm steel ball falls needed for 20cm from described viscose solution) 45s, degree of ripeness (10%NH
4cl) 9.4ml, is stand-by viscose solution.
The preparation of precrosslink krill protein solution: preparing mass fraction with distilled water in reactor is the sodium hydroxide solution of 3%, the krill albumen that weight is sodium hydroxide solution 5% is added in reactor, in still, add the dispersant sulfomethylated lignin acid amide that weight is krill albumen 0.3% again, when its effect is and prevents krill albumen from falling at temperature, bulk can be become to separate out.Stir 4 hours at 50 DEG C, to be cooled to temperature to 35 DEG C insulation filtration, collect filtrate and filter residue, gained filtrate is krill protein solution.In gained krill protein solution, add the glutaraldehyde that weight is krill albumen 1% again, 35 DEG C of insulation reaction 0.5h, prepare precrosslink krill protein solution.
Viscose solution mixes with the grafting of protein solution:
(1) first above-mentioned krill protein solution is cooled to 28 DEG C-30 DEG C, insulation deaeration;
(2) by spinning front injection measurement pump, be injected into by a certain percentage in the viscose glue of deaeration completely, blended viscose fully mixes respectively through dynamic mixer and static mixer, finally sends into spinning, and whole process completes within 4min.
(3) described in above-mentioned steps (2), certain proportion is as follows: krill protein solution adopts syringe pump with the speed injection of 5.25kg/min in dynamic mixer, crosslinking agent glutaraldehyde adopts syringe pump with the speed injection of 0.24kg/min in dynamic mixer, make it mix with viscose solution, the flow of viscose solution is 294.3kg/min.In obtained mixed solution, content of crosslinking agent is 1%, and krill protein content is 2%, the fine content 8.9% of first.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 52m/min, and coagulation bath temperature is 49 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 120g/L, sodium sulphate 325g/L, zinc sulfate 12g/L.
embodiment 2
The preparation of viscose solution: the Cotton Pulp adopting the fine mass content 93.5% of the degree of polymerization 500, first, successively through dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, the operation such as deaeration prepare spinning viscose solution.Fine mass content 8.9%, the NaOH mass content 5.5% of obtained first, viscosity (falling ball method) 50s, degree of ripeness (10%NH
4cl) 9.2ml, is stand-by viscose solution.
The preparation of precrosslink krill protein solution: preparing mass fraction with distilled water in reactor is the sodium hydroxide solution of 7%, the krill albumen that weight is sodium hydroxide solution 13% is added in reactor, in still, add the dispersant sulfomethylated lignin acid amide that weight is krill albumen 0.7% again, when its effect is and prevents krill albumen from falling at temperature, bulk can be become to separate out.Stir 5 hours at 60 DEG C, to be cooled to temperature to 40 DEG C insulation filtration, collect filtrate and filter residue, gained filtrate is krill protein solution.In gained krill protein solution, add the ethylene glycol diglycidylether that weight is krill albumen 1.5% again, 40 DEG C of insulation reaction 0.5h, prepare precrosslink krill protein solution.
Viscose solution mixes with the grafting of protein solution:
(1) first above-mentioned krill protein solution is cooled to 28 DEG C-30 DEG C, insulation deaeration;
(2) by spinning front injection measurement pump, be injected into by a certain percentage in the viscose solution of deaeration completely, blended viscose fully mixes respectively through dynamic mixer and static mixer, finally sends into spinning, and whole process completes within 7min.
(3) described in above-mentioned steps (2), certain proportion is as follows: krill protein solution adopts syringe pump with the speed injection of 12.43kg/min in dynamic mixer, crosslinking agent ethylene glycol diglycidylether adopts syringe pump with the speed injection of 2.56kg/min in dynamic mixer, make it mix with viscose solution, the flow of viscose solution is 448kg/min.In obtained mixed solution, content of crosslinking agent is 7%, and krill protein content is 4%, the fine content 8.9% of first.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 52m/min, and coagulation bath temperature is 50 DEG C, and plasticizing-bath temperature is 98 DEG C.Coagulation bath composition is: sulfuric acid 125g/L, sodium sulphate 330g/L, zinc sulfate 14g/L.
embodiment 3
The preparation of viscose solution: the Cotton Pulp adopting the fine mass content 93.5% of the degree of polymerization 500, first, successively through dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, the operation such as deaeration prepare spinning viscose solution.Fine mass content 8.9%, the NaOH mass content 5.5% of obtained first, viscosity (falling ball method) 48s, degree of ripeness (10%NH
4cl) 9.1ml, is stand-by viscose solution.
The preparation of precrosslink krill protein solution: preparing mass fraction with distilled water in reactor is the sodium hydroxide solution of 10%, the krill albumen that weight is sodium hydroxide solution 20% is added in reactor, the dispersant sulfomethylated lignin acid amide that weight is krill albumen 1% is added again in still, add in reactor and account for the krill albumen that solution quality is 20%, add in still again and account for the dispersant sulfomethylated lignin acid amide that krill albumen quality percentage is 1%, when its effect is and prevents krill albumen from falling at temperature, bulk can be become to separate out.Stir 6 hours at 70 DEG C, to be cooled to temperature to 45 DEG C insulation filtration, collect filtrate and filter residue, gained filtrate is krill protein solution.In gained krill protein solution, add the glutaraldehyde and 0.5% polyethyleneglycol diglycidylether that weight is krill albumen 1.5% again, 45 DEG C of insulation reaction 0.5h, prepare precrosslink krill protein solution.
Viscose solution mixes with the grafting of protein solution:
(1) first above-mentioned krill protein solution is cooled to 28 DEG C-30 DEG C, insulation deaeration;
(2) by spinning front injection measurement pump, be injected into by a certain percentage in the viscose solution of deaeration completely, blended viscose fully mixes respectively through dynamic mixer and static mixer, finally sends into spinning, and whole process completes within 10min.
(3) described in above-mentioned steps (2), certain proportion is as follows: krill protein solution adopts syringe pump with the speed injection of 15.54kg/min in dynamic mixer, crosslinking agent glutaraldehyde and polyethyleneglycol diglycidylether adopt syringe pump with the speed injection of 6.00kg/min in dynamic mixer, make it mix with viscose solution, the flow of viscose solution is 612.6kg/min.In obtained mixed solution, content of crosslinking agent is 12%, and krill protein content is 8%, the fine content 8.9% of first.
Wet spinning: the mixed solution of precrosslink protein and viscose glue is sent into wet spinning operation and carries out spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 52m/min, and coagulation bath temperature is 49 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 120g/L, sodium sulphate 325g/L, zinc sulfate 12g/L.
Leading indicator through the obtained fiber of embodiment 1 ~ 3 is as follows:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Protein content (%) | 1.68 | 3.28 | 6.24 |
| Albumen retention rate (%) | 84 | 82 | 78 |
| Fiber number (dtex) | 1.59 | 1.68 | 1.63 |
| Dry strong (cN/ dtex) | 2.01 | 2.23 | 2.18 |
| Wet strong (cN/ dtex) | 1.12 | 1.32 | 1.21 |
| Dryly to stretch (%) | 17.6 | 18.2 | 20.5 |
Note: 1, evaluate according in table 2 in FZ/T54028-2010 " cotton protein viscose staple fibre performance project and desired value ", wherein dry fracture strength has reached the high-class product rank in standard, meets the requirements completely.
2, evaluate according in table 2 in FZ/T54028-2010 " cotton protein viscose staple fibre performance project and desired value ", by both sides of supply and demand determination protein content central value, the protein content produced, meets the requirements completely.And the retention rate of albumen on fiber is also higher.
Claims (5)
1. a preparation method for krill protein renaturation cellulose fibre, is characterized in that: comprise the following steps;
Step (1), Making viscose solution, for subsequent use;
Step (2), preparation precrosslink krill protein solution: add sodium hydroxide solution, krill albumen and sulfomethylated lignin acid amide in a reservoir successively, at 50-70 DEG C, stir 4-6 hour, be cooled to 35-45 DEG C of insulation and filter, gained filtrate is krill protein solution; In krill protein solution, add crosslinking agent, at 35-45 DEG C of insulation reaction 0.4-0.6h, prepare precrosslink krill protein solution; The weight of the krill albumen added is the 5-20% of sodium hydroxide solution weight, and the weight that sulfomethylated lignin acid amide adds is the 0.3-1% of krill protein by weight, and the weight that crosslinking agent adds is the 1-2% of krill protein by weight;
Step (3), by viscose solution, precrosslink krill protein solution, crosslinking agent mixing after spinning, dosage of crosslinking agent is 1 ~ 12% of the fine mass content of first in viscose solution, and in described precrosslink krill protein solution, the weight of krill albumen is 1 ~ 8% of the fine weight of first in rayon spinning stoste.
2. the preparation method of krill protein renaturation cellulose fibre according to claim 1, is characterized in that: the mass fraction of step (2) sodium hydroxide solution is 3-10%.
3. the preparation method of krill protein renaturation cellulose fibre according to claim 1, is characterized in that: crosslinking agent is one or more in glutaraldehyde, ethylene glycol diglycidylether, polyethyleneglycol diglycidylether.
4. the preparation method of krill protein renaturation cellulose fibre according to claim 1, is characterized in that: adopt the method for dynamically mixing and static mixing to mix during step (3) spinning.
5. the preparation method of krill protein renaturation cellulose fibre according to claim 1, is characterized in that: step (3) completes within 10 minutes from the whole process being mixed into spinning.
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| CN104451930B (en) * | 2014-11-20 | 2017-07-14 | 江苏金太阳纺织科技股份有限公司 | A kind of preparation method of whisker reinforcement regenerated celulose fibre |
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| CN102808239A (en) * | 2012-08-24 | 2012-12-05 | 东北林业大学 | Method for preparing chitin nano filaments |
| CN102926025A (en) * | 2012-11-14 | 2013-02-13 | 大连工业大学 | Preparation method of synthetic wig fiber |
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| CN102808239A (en) * | 2012-08-24 | 2012-12-05 | 东北林业大学 | Method for preparing chitin nano filaments |
| CN102926025A (en) * | 2012-11-14 | 2013-02-13 | 大连工业大学 | Preparation method of synthetic wig fiber |
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Address after: 226314 Jiangsu city of Nantong province Tongzhou District Industrial Park building sun Zhihao Patentee after: JIANGSU GOLDSUN TEXTILE TECHNOLOGY CO., LTD. Address before: 226314 Jiangsu city of Nantong province Tongzhou District Industrial Park building sun Zhihao Patentee before: Goldsun Holding Group Co., Ltd. |