CN1546781A - Composite hydrosol color fixing finishing agent, synthesizing method and use thereof - Google Patents
Composite hydrosol color fixing finishing agent, synthesizing method and use thereof Download PDFInfo
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- CN1546781A CN1546781A CNA2003101091194A CN200310109119A CN1546781A CN 1546781 A CN1546781 A CN 1546781A CN A2003101091194 A CNA2003101091194 A CN A2003101091194A CN 200310109119 A CN200310109119 A CN 200310109119A CN 1546781 A CN1546781 A CN 1546781A
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Abstract
The invention refers to a kind of compound lyosol fixing arrangement agent, a synthesizing method and the usage. The arrangement agent is made up of following products: (1) the silicon sol is made up of gamma-glycidol ether oxygen propyl trimethoxy-silane, water and hydrochloric acid, whose mol proportion is: 1:5-100:1x10 -5-1x10 -1; (2) the titanium sol is made up of titanic acid butyl ester, water and hydrochloric acid whose proportion is 1:0.1-10:10-200: 1x10 -4-1x10 -1; (3) the product is produced by mixing above mentioned silicon sol and titanium sol, the mol proportion of silicon and titanium is 1:0.05-1.0. The arrangement agent may form a mesh particle film on the surface of the fiber, realizes the color fixing aim.
Description
Technical field
The present invention relates to a kind of DYED FABRICS post-finishing agent, specifically a kind of Compound Hydrosol Fixation Finishing Agent, preparation method and use.
Background technology
Sol-gel process is that the organic or inorganic compound with metal forms colloidal sol through hydrolysis, makes the colloidal sol polymeric gelization then, again with gel drying, bake, become the method for oxide or other solid chemical compound.As a kind of preparation methods, sol-gal process can be traced back in the middle of the 19th century, and through 100 years of development, this method is applied in various fields, is mainly used at present preparing on glass, superfine powder and the film.In preparation process, to adopt 300～800 ℃ high-temperature roasting.When the system film, adopt smooth surfaces such as glass, metal, plastics to carry out coating, form reticular membrane in stromal surface, to give material surface brand-new character as matrix.The application of sol-gel process in weaving is just at the early-stage, because textiles can't bear high-temperature roasting, and its surface is hackly, therefore has many difficulties aspect textile finishing.We have solved all technical problems through concentrating on studies, and sol-gel technique is applied to textiles (publication number CN1425825A, application number 03114856.5).This patent is selected for use and with textiles chemically combined reagent can be taken place and make feedstock production colloidal sol, adopts the finishing technique that pads-bake this suitable textiles, textiles is carried out suitable processing after, can improve the COLOR FASTNESS of textiles, but also have following shortcoming:
(1) when preparation colloidal sol, adopts the cosolvent of ethanol, contain a large amount of ethanol in the colloidal sol that makes, be unfavorable for industrial production as silane and water;
(2) prepared colloidal sol has good colour fixation to direct fast black G, but not too obvious to the colour fixation of other direct dyes.
The present invention adopts water as solvent, prepare Ludox and titanium colloidal sol respectively, the fixation treatment that the two is used for DYED FABRICS after compound according to a certain percentage, a plurality of direct dyes there is good colour fixation, reactive and ACID DYES also there is colour fixation preferably, be a kind of effective color-fixing method, can reduce washes, alleviate pollution environment.
Summary of the invention:
The purpose of this invention is to provide a kind of Compound Hydrosol Fixation Finishing Agent, is to be composited by Ludox and titanium colloidal sol.
Another object of the present invention provides a kind of synthetic method of above-mentioned finishing agent, this method is solvent with water, selecting γ-glycidyl ether oxygen propyl trimethoxy silicane (GPTS), butyl titanate (TTB) for use is raw material, at room temperature prepare Ludox and titanium colloidal sol respectively, be composited by a certain percentage then.
Purpose of the present invention also provides a kind of purposes of above-mentioned finishing agent.Promptly adopt finishing agent of the present invention that fabric is carried out padding finishing,, form the thin and transparent film that constitutes by silicon titanium composite network structure, dyestuff on the fabric is carried out fixation at fiber surface again through heat treatment.
Compound Hydrosol Fixation Finishing Agent of the present invention is to be made up of following product:
Ludox:
γ-glycidyl ether oxygen propyl trimethoxy silicane: water: hydrochloric acid=1: 5～100: 1 * 10
-5～1 * 10
-1
Titanium colloidal sol:
Butyl titanate: acetic acid: water: hydrochloric acid=1: 0.1～10: 10～200: 1 * 10
-4～1 * 10
-1
Compound Hydrosol Fixation Finishing Agent:
Mixed by above-mentioned Ludox and titanium colloidal sol, the mol ratio of silicon and titanium is 1: 0.05～1.0, and recommending mol ratio is 1: 0.1～0.5.
Above ratio is mol ratio.
Concrete synthetic method is as follows:
1. the preparation of the siliceous hydrosol
GPTS and water are joined in the beaker, drip dilute hydrochloric acid solution under the magnetic agitation, drip off the back and stir the siliceous hydrosol that can obtain clear in 10-50 minute.
2. the preparation of the titaniferous hydrosol
TTB is dissolved in the acetum, under magnetic agitation, the acetum of TTB is splashed in the distilled water that contains watery hydrochloric acid then, stir and obtain milky white liquid after 10-50 minute, this liquid is transferred in the separatory funnel, the ageing certain hour takes off a layer translucent liquid and is the titaniferous hydrosol.
3. the preparation of the compound hydrosol of Si/Ti
According to 1. and the method 2. prepare the siliceous hydrosol and the hydrosol of titaniferous respectively, according to silicon/titanium 1: 0.05～1.0 mol ratio ratios, recommending silicon/titanium mol ratio is 1: 0.1～0.5, under magnetic agitation, slowly the latter is added drop-wise among the former, promptly obtains the compound hydrosol of Si/Ti after stirring.
Concrete method for sorting is as follows:
With the siliceous hydrosol and the titaniferous hydrosol compound according to a certain percentage after, will dye good cloth and in the compound hydrosol, two soak two and roll pressure 2～3kg/cm
2, liquid carrying rate about 60～80%.Cloth 60-80 ℃ of oven dry in convection oven with after the arrangement baked 3～5 minutes at 150～170 ℃ then.
Adopt above-mentioned finishing technique, can form the thin and transparent gel mould of one deck on the surface of fiber at a lower temperature, fixed dye molecule, the COLOR FASTNESS of raising dyestuff.
Compare with traditional color-fixing agent, the dressing liquid among the present invention has the following advantages:
1. for dyestuff universality is arranged, promptly inhomogeneous dyestuffs such as direct, reactivity, acidity are all had good tint retention;
2. formaldehydeless;
3. look diminishes;
4. form firm combining between complex sol and the textiles, every COLOR FASTNESS is improved greatly;
5. significantly reduce the washes after the dyeing, alleviate pollution environment.
Compare with last applying for a patent (publication number CN1425825A, application number 03114856.5), the present invention has the following advantages:
1. adopt water as solvent fully,, more be suitable for actual production than containing alcohol solvent more economically;
2. the siliceous hydrosol and the titaniferous hydrosol is compound according to a certain percentage, can form more fine and close gel mould at fiber surface, colour fixation is better;
3. the compound hydrosol of the present invention all has more significant colour fixation to a plurality of direct dyes that comprise direct fast black G;
4. the compound hydrosol among the present invention is more obvious to the colour fixation of chemically-reactive dyes and ACID DYES.
The specific embodiment:
(1) use respectively many direct dyes, chemically-reactive dyes and ACID DYES to the plain weave cotton poplin (density: 133/72, number 40 * 40,120g/m
2) dyeing.
(2) according to γ-glycidyl ether oxygen propyl trimethoxy silicane: water: hydrochloric acid=1: 5～100: 1 * 10
-5～1 * 10
-1Molar ratio, GPTS and water are joined in the beaker, drip dilute hydrochloric acid solution under the magnetic agitation, stir the siliceous hydrosol that can obtain clear behind the certain hour.
(3) according to butyl titanate: acetic acid: water: hydrochloric acid=1: 0.1～10: 10～200: 1 * 10
-4～1 * 10
-1Molar ratio, TTB is dissolved in the acetum, under magnetic agitation, the acetum of TTB is added dropwise in the distilled water that contains watery hydrochloric acid then, obtain milky white liquid after stirring certain hour, this liquid is transferred in the separatory funnel, the ageing certain hour takes off a layer translucent liquid and is the titaniferous hydrosol.
(4) prepare the siliceous hydrosol and the hydrosol of titaniferous according to (2), (3),, under magnetic agitation, slowly the latter is added drop-wise among the former, promptly obtain the compound hydrosol of Si/Ti after stirring according to certain silicon/titanium ratio.
(5) with the siliceous hydrosol and the titaniferous hydrosol compound according to a certain percentage after, will dye good cloth and in the compound hydrosol, two soak two and roll pressure 2～3kg/cm
2, liquid carrying rate about 60～80%.Cloth 60-80 ℃ of oven dry in convection oven with after the arrangement baked 3～5 minutes at 150～170 ℃ then.
(6) with reference to GB3921-83, GB3920-83, GB6152-85 the cloth specimen before and after the arrangement is tested soaping fastness, crock fastness and the wet fastness of scalding respectively, use Datacolor SF600
+Color measurement and color match instrument evaluation progression, each cloth specimen test three times is averaged.
The preparation of the embodiment 1. compound hydrosols
1. according to γ-glycidyl ether oxygen propyl trimethoxy silicane: water: hydrochloric acid=1: 20: 3 * 10
-5Ratio, GPTS and water are joined in the beaker, drip dilute hydrochloric acid solution under the magnetic agitation, the room temperature lower magnetic force stirred 30 minutes, can obtain the siliceous hydrosol of clear.
2. according to butyl titanate: acetic acid: water: hydrochloric acid=1: 2.5: 50: 0.014 ratio, TTB is dissolved in the acetum, under magnetic agitation, the acetum of TTB is added dropwise in the distilled water that contains watery hydrochloric acid then, stir under the room temperature and obtained milky white liquid in 30 minutes, this liquid is transferred in the separatory funnel, ageing 1 hour is taken off a layer translucent liquid and is the titaniferous hydrosol.
3. according to Si/Ti=5: the ratio of 1 (mol ratio), under magnetic agitation, slowly the titaniferous hydrosol is added drop-wise in the siliceous hydrosol, promptly obtain the compound hydrosol of Si/Ti after stirring.
Embodiment 2. direct dyes fixation
Use Solophenyl Blue RL (Ciba) respectively, Solophenyl Yellow FFL (Ciba), IndosolBubine SF-RGN (Clarient), Turquoise FBL (inspiring confidence in Dye Co., Ltd in the Taiwan), Rose FR (inspiring confidence in Dye Co., Ltd in the Taiwan), the dye liquor of Direct Black G (dyestuff factory, Tongxiang, Zhejiang) preparation 2% (o.w.f), the glauber salt consumption is 25g/l, bath raio 1: 20.40 ℃ are dyed, and add 1/2 glauber salt and dyestuff, and the speed with 1 ℃/min after 10 minutes is warming up to 98 ℃, add residue 1/2 glauber salt after 5 minutes, dye and are cooled to 80 ℃ after 40 minutes, clean with clear water after taking out.
The compound hydrosol with embodiment 1 gained is put in order DYED FABRICS, and the data of the soaping fastness of six direct dyes, crock fastness and wet boiling hot fastness were as shown in table 1 before and after sol-gel process was handled:
Every COLOR FASTNESS contrast before and after the table 1 direct dyes fixation treatment
| Dyestuff | Soaping fastness | Crock fastness | The wet fastness of scalding | ||||
| The former state variable color | Calico staining | Unlubricated friction | Wet rubbing | The former state variable color | Calico staining | ||
| ???Solophenyl?Blue?RL | Before the processing | 4-5 | 1-2 | ?5 | ?3 | ?5 | ?3 |
| After the processing | 4-5 | 3-4 | ?5 | ?4 | ?4-5 | ?4 | |
| ??Solophenyl?Yellow?FFL | Before the processing | 4 | 1-2 | ?5 | ?3 | ?4-5 | ?3-4 |
| After the processing | 2-3 | 2 | ?5 | ?4-5 | ?4-5 | ?4-5 | |
| ?Indosol?Bubine?SF-RGN | Before the processing | 4-5 | 1-2 | ?5 | ?3 | ?4-5 | ?4 |
| After the processing | 4 | 4 | ?5 | ?4 | ?3 | ?5 | |
| ?????Turquoise?FBL | Before the processing | 2-3 | 2-3 | ?4-5 | ?1-2 | ?2-3 | ?2-3 |
| After the processing | 2 | 3-4 | ?5 | ?4 | ?2-3 | ?4-5 | |
| ????????Rose?FR | Before the processing | 4-5 | 1-2 | ?5 | ?2-3 | ?5 | ??2 |
| After the processing | 4-5 | 3-4 | ?5 | ?4-5 | ?4 | ?4-5 | |
| ?????Direct?Black?G | Before the processing | 4 | 1-2 | ?4-5 | ?2-3 | ?4-5 | ?2 |
| After the processing | 3-4 | 3-4 | ?5 | ?4-5 | ?4-5 | ?4-5 | |
Annotate: the former state variable color progression decline of handling in the soaping fastness of back is because the back cloth specimen of soaping has " washing increases deeply "
Effect causes.
Embodiment 3. chemically-reactive dyes fixation
Use the dye liquor of active emerald green blue B-BEFN, reactive scarlet B-3G, active emerald green blue BES, reactive scarlet BES (Shanghai Wande Chemical Co., Ltd.) preparation 2% (o.w.f) respectively, the glauber salt consumption is 40g/l, and the sodium carbonate consumption is 20g/l, bath raio 1: 20.60 ℃ of constant temperature dyeings rise and dye adding 1/2 glauber salt and dyestuff after 10 minutes, add residue 1/2 glauber salt after 10 minutes, add sodium carbonate after 10 minutes again, be cooled to 40 ℃ after 30 minutes, take out, boil with 1g/l neutral detergent solution and boil 1 minute in the washing back, cloth is dried in fully washing then.
The compound hydrosol with embodiment 1 gained is put in order DYED FABRICS, and the data of the soaping fastness of four chemically-reactive dyess, crock fastness and wet boiling hot fastness were as shown in table 2 before and after sol-gel process was handled:
Every COLOR FASTNESS contrast before and after the table 2 chemically-reactive dyes fixation treatment
| Dyestuff | Soaping fastness | Crock fastness | The wet fastness of scalding | ||||
| The former state variable color | Calico staining | Unlubricated friction | Wet rubbing | The former state variable color | Calico staining | ||
| Active emerald green blue B-BEFN | Before the processing | 3 | 2-3 | ?5 | ?4 | ?4-5 | 4-5 |
| After the processing | 4-5 | 3 | ?5 | ?4-5 | ?5 | 5 | |
| Reactive scarlet B-3G | Before the processing | 4-5 | 3-4 | ?5 | ?4 | ?4-5 | 4 |
| After the processing | 4-5 | 4-5 | ?5 | ?4-5 | ?4-5 | 5 | |
| Active emerald green blue BES | Before the processing | 3-4 | 2-3 | ?5 | ?4 | ?4-5 | 4-5 |
| After the processing | 4 | 3 | ?5 | ?4-5 | ?4-5 | 5 | |
| Reactive scarlet BES | Before the processing | 4-5 | 4-5 | ?5 | ?4-5 | ?4-5 | 4 |
| After the processing | 4-5 | 4-5 | ?5 | ?4-5 | ?4-5 | 4-5 | |
Embodiment 4. ACID DYES fixation
Use Lanasan Red CF-A (Clarient) and Erionyl Red A-2BF (Ciba) to cotton fabric dyeing process respectively, the dye liquor of preparation 5% (o.w.f) is adjusted to PH=4-6 with glacial acetic acid, according to the dyeing dyeing (referring to embodiment 2) of direct dyes.Dye good back without washing, (liquid carrying rate 60-70%) is 60 ℃ of oven dry after the pressure rolling.
The compound hydrosol with embodiment 1 gained is put in order DYED FABRICS, and the data of the soaping fastness of two ACID DYES, crock fastness and wet boiling hot fastness were as shown in table 3 before and after sol-gel process was handled:
The soaping fastness before and after the table 3 ACID DYES fixation treatment and the waste liquid absorbance contrast of soaping
| Dyestuff | Soaping fastness | Waste liquid absorbance after soaping | ||
| The former state variable color | Calico staining | |||
| ????Lanasan?Red?CF-A | Before the processing | ????1 | ????4 | ????1.411 |
| After the processing | ????4 | ????5 | ????0.256 | |
| ?Ciba?Erionyl?Red?A-2BF | Before the processing | ????1 | ????2 | ????2.197 |
| After the processing | ????3-4 | ????3 | ????0.801 | |
Claims (7)
1, a kind of Compound Hydrosol Fixation Finishing Agent, form by following product:
(1) Ludox of being made up of γ-glycidyl ether oxygen propyl trimethoxy silicane, water and hydrochloric acid, their mol ratio is respectively 1: 5～100: 1 * 10
-5～1 * 100
-1
(2) form titanium colloidal sol by butyl titanate, acetic acid, water and hydrochloric acid, their mole is respectively 1: 0.1～10: 10～200: 1 * 10
-4～1 * 10
-1
(3) mixed by above-mentioned Ludox and titanium colloidal sol, wherein the mol ratio of silicon and titanium is 1: 0.05～1.0.
2, a kind of Compound Hydrosol Fixation Finishing Agent as claimed in claim 1 is characterized in that wherein the mol ratio of silicon and titanium is 1: 0.05～1.0.
3, the synthetic method of Compound Hydrosol Fixation Finishing Agent as claimed in claim 1 is characterized in that adopting following method synthetic:
(1) at room temperature watery hydrochloric acid is added dropwise in γ-glycidyl ether oxygen propyl trimethoxy silicane and the water, stir into the Ludox of clear, the mol ratio of described γ-glycidyl ether oxygen propyl trimethoxy silicane, water and hydrochloric acid is followed successively by 1: 5～100: 1 * 10
-5～1 * 10
-1
(2) acetum that will dissolve butyl titanate under the room temperature is added dropwise in the watery hydrochloric acid, stirs the titanium colloidal sol of the liquid that is creamy white, and wherein the mol ratio of butyl titanate, acetic acid, water and hydrochloric acid is 1: 0.1～10: 10～200: 1 * 10
-4～1 * 10
-1
(3) the titanium colloidal sol of (2) is under agitation splashed in the Ludox of (1) in room temperature and under stirring, wherein the mol ratio of silicon and titanium is 1: 0.05～1.0.
4, synthetic method as claimed in claim 3, the mol ratio that it is characterized in that described silicon and titanium is 1: 0.01～0.5.
5, synthetic method as claimed in claim 3, the mol ratio that it is characterized in that described silicon and titanium is 1: 0.1-1.0.
6, synthetic method as claimed in claim 3 is characterized in that the wherein titanium colloidal sol described in the method (2), takes off a layer translucent liquid after ageing.
7, a kind of purposes of Compound Hydrosol Fixation Finishing Agent as claimed in claim 1 is characterized in that being used for the fixing finish after the dyeing of cellulose fiber fiber products.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109119 CN1282794C (en) | 2003-12-05 | 2003-12-05 | Composite hydrosol color fixing finishing agent, synthesizing method and use thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109119 CN1282794C (en) | 2003-12-05 | 2003-12-05 | Composite hydrosol color fixing finishing agent, synthesizing method and use thereof |
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|---|---|
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| CN1282794C CN1282794C (en) | 2006-11-01 |
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|---|---|---|---|
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|---|---|---|---|---|
| CN100363437C (en) * | 2006-01-06 | 2008-01-23 | 浙江大学 | Method for preparing silicon-titanium micro-coarse structured hydrophilic film |
| CN100412261C (en) * | 2006-06-30 | 2008-08-20 | 东华大学 | Modified silane sol with amino silicone oil emulsion and its preparation process and usage |
| CN100458003C (en) * | 2006-07-02 | 2009-02-04 | 刘祥 | Organic nanometer spinning paste adjuvant composition and its synthesis method |
| CN101349015B (en) * | 2007-10-26 | 2011-03-16 | 江南大学 | Preparation and application of colloidal sol dyeing liquor |
| CN102912661A (en) * | 2012-11-07 | 2013-02-06 | 愉悦家纺有限公司 | Fixation treating method for fabric |
| CN102965912A (en) * | 2012-11-20 | 2013-03-13 | 江南大学 | Preparation method of alkaline reaction type silicon-titanium collosol applicable to thermal transfer printing of cotton fabric |
| CN103572621A (en) * | 2013-11-15 | 2014-02-12 | 东华大学 | Method for improving color fastness of photochromic fabric |
| CN103911877A (en) * | 2014-04-17 | 2014-07-09 | 傅科杰 | Color-changing agent applicable to textile fabrics |
| CN104047192A (en) * | 2014-06-10 | 2014-09-17 | 盐城市印染有限公司 | Color-fixing anti-wrinkle finishing agent as well as preparation method and application thereof |
| CN106758411A (en) * | 2016-12-07 | 2017-05-31 | 郑州源冉生物技术有限公司 | A kind of alkaline-resisting environmentally friendly color fixing agent of activity and preparation method thereof |
| CN109054507A (en) * | 2018-07-20 | 2018-12-21 | 中南林业科技大学 | Alkaline titanium colloidal sol color fixing agent and its preparation method and application |
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| CN100363437C (en) * | 2006-01-06 | 2008-01-23 | 浙江大学 | Method for preparing silicon-titanium micro-coarse structured hydrophilic film |
| CN100412261C (en) * | 2006-06-30 | 2008-08-20 | 东华大学 | Modified silane sol with amino silicone oil emulsion and its preparation process and usage |
| CN100458003C (en) * | 2006-07-02 | 2009-02-04 | 刘祥 | Organic nanometer spinning paste adjuvant composition and its synthesis method |
| CN101349015B (en) * | 2007-10-26 | 2011-03-16 | 江南大学 | Preparation and application of colloidal sol dyeing liquor |
| CN102912661A (en) * | 2012-11-07 | 2013-02-06 | 愉悦家纺有限公司 | Fixation treating method for fabric |
| CN102912661B (en) * | 2012-11-07 | 2015-03-18 | 愉悦家纺有限公司 | Fixation treating method for fabric |
| CN102965912B (en) * | 2012-11-20 | 2016-05-25 | 江南大学 | Be suitable for cotton type fabric thermal transfer printing alkaline reaction type silicon titanium colloidal sol preparation method |
| CN102965912A (en) * | 2012-11-20 | 2013-03-13 | 江南大学 | Preparation method of alkaline reaction type silicon-titanium collosol applicable to thermal transfer printing of cotton fabric |
| CN103572621A (en) * | 2013-11-15 | 2014-02-12 | 东华大学 | Method for improving color fastness of photochromic fabric |
| CN103911877A (en) * | 2014-04-17 | 2014-07-09 | 傅科杰 | Color-changing agent applicable to textile fabrics |
| CN104047192A (en) * | 2014-06-10 | 2014-09-17 | 盐城市印染有限公司 | Color-fixing anti-wrinkle finishing agent as well as preparation method and application thereof |
| CN106758411A (en) * | 2016-12-07 | 2017-05-31 | 郑州源冉生物技术有限公司 | A kind of alkaline-resisting environmentally friendly color fixing agent of activity and preparation method thereof |
| CN109054507A (en) * | 2018-07-20 | 2018-12-21 | 中南林业科技大学 | Alkaline titanium colloidal sol color fixing agent and its preparation method and application |
| CN109054507B (en) * | 2018-07-20 | 2022-07-19 | 中南林业科技大学 | Alkaline titanium sol color fixing agent and preparation method and application thereof |
| CN110172842A (en) * | 2019-04-09 | 2019-08-27 | 于洪波 | A kind of silk gradient color dyeing and printing process |
| CN110565369A (en) * | 2019-09-27 | 2019-12-13 | 南通大学 | Treatment method for improving fastness to soaping and fading of yarn dyed fabric and yarn dyed fabric |
| CN110565369B (en) * | 2019-09-27 | 2022-01-21 | 南通大学 | Treatment method for improving fastness to soaping and fading of yarn dyed fabric and yarn dyed fabric |
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| C14 | Grant of patent or utility model | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Shanghai New Iron Chain Bolting Cloth Manufacturing Co., Ltd. Assignor: Donghua University Contract fulfillment period: 2006.12.1 to 2011.12.31 contract change Contract record no.: 2008310000107 Denomination of invention: Composite hydrosol color fixing finishing agent, synthesizing method and use thereof Granted publication date: 20061101 License type: Exclusive license Record date: 2008.10.6 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.12.1 TO 2011.12.31; CHANGE OF CONTRACT Name of requester: SHANGHAI XINTIELIAN SIEVE MANUFACTURING CO., LTD. Effective date: 20081006 |
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Granted publication date: 20061101 Termination date: 20121205 |