CN105256568A - Application of ecological auxiliary to woolen sweater finishing - Google Patents
Application of ecological auxiliary to woolen sweater finishing Download PDFInfo
- Publication number
- CN105256568A CN105256568A CN201510770772.8A CN201510770772A CN105256568A CN 105256568 A CN105256568 A CN 105256568A CN 201510770772 A CN201510770772 A CN 201510770772A CN 105256568 A CN105256568 A CN 105256568A
- Authority
- CN
- China
- Prior art keywords
- agent
- woollen sweater
- weight
- oven dry
- auxiliary agent
- 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
Links
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses application of an ecological auxiliary to woolen sweater finishing. According to the application, the ecological auxiliary is prepared; an agent B is sprayed to a woolen sweater uniformly, the spraying weight is 0.1 time that of the woolen sweater, and the woolen sweater is placed for 12-15 hours in a closed mode at the temperature of 25 DEG C-28 DEG C, and dried at the temperature of 30 DEG C for use; then an agent A is sprayed to the dried woolen sweater uniformly, the spraying weight is 0.05-0.08 time that of the woolen sweater, the woolen sweater stands for 350-420 minutes at the temperature of 35 DEG C-39 DEG C, and is dried at the temperature of 30 DEG C, and the constant temperature and ventilation are kept in the standing process; deionized water is used for cleaning residues on the surface of fabric, and the fabric is baked for 5 s at the temperature of 60 DEG C and then dried at the temperature of 30 DEG C.
Description
Technical field
The present invention relates to the application of a kind of ecological auxiliary agent on woollen sweater arranges, belong to textile technology field.
Background technology
Woollen sweater is raw material with sheep's wool, and be the most popular sweater knitted, its needle path is clear, shirt face is bright and clean, fat light foot, bright color, good hand feeling high resilience; Woollen sweater is more endurable, moderate, but feel is more far short of what is expected than woollen sweater, and class is also much lower.
Afterfinish method is the key factor affecting wool pin performance.Along with the raising day by day of living standard, the health care consciousness of people to textile garment strengthens day by day, has the knitwear wide market next to the skin of anti-microbial property.Antibacterial fabric processing is main adopts 2 kinds of technological approaches: one is add antiseptic before fibre spinning is shaped, and carries out modification and obtains anti-bacterial fibre; Two is use antiseptic, by padding, flood, coating, the method finish fabric such as spraying, and acquisition antibacterial effect.Direct its durable antibacterial effect of employing anti-bacterial fibre, but be only applicable to synthetic fiber and regenerated fiber, technical requirement is high, complicated operation, and cost is higher.Use antibacterial finishing agent is simple and convenient, and be applicable to most of fiber textile, cost is low, but whether the persistence of anti-microbial property can be guaranteed, and whether affects the wearability of fabric, has become the problem of insider's primary study.
The present invention aims to provide the application of a kind of ecological auxiliary agent on woollen sweater arranges, and described ecological auxiliary agent comprises compound live bacteria agent, native protein, natural polysaccharide etc., not containing any chemical reagent, use simple, the woollen sweater after arrangement has good antibacterial effect, and can also ANTIPILLING, make the feel of woollen sweater finer and smoother, have gloss, mechanical strength strengthens, upper dye, on whiteness then without any impact.
Summary of the invention
Based on the technical problem that background technology exists, the invention provides the application of a kind of ecological auxiliary agent on woollen sweater arranges, described ecological auxiliary agent comprises compound live bacteria agent, native protein, natural polysaccharides etc., not containing any chemical reagent, use simple, woollen sweater after arrangement has good antibacterial effect, and can also ANTIPILLING, makes the feel of woollen sweater finer and smoother, there is gloss, mechanical strength strengthens, upper dye, on whiteness then without any impact.
Technical scheme of the present invention is as follows:
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1-1.5*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.0-1.5%, pigskin collagen 0.6=0.9%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 25-28 DEG C puts 12-15 hour, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.05-0.08 times of the weight of woollen sweater, leaves standstill 350-420min at being then placed in 35-39 DEG C, dries in the processes of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Usefulness of the present invention is:
The invention provides the application of a kind of ecological auxiliary agent on woollen sweater arranges, described ecological auxiliary agent comprises compound live bacteria agent, native protein, natural polysaccharide etc., not containing any chemical reagent, use simple, the woollen sweater after arrangement has good antibacterial effect, and can also ANTIPILLING, make the feel of woollen sweater finer and smoother, have gloss, mechanical strength strengthens, upper dye, on whiteness then without any impact.
Detailed description of the invention
Embodiment 1:
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.5%, pigskin collagen 0.6%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 28 DEG C puts 12 hours, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.08 times of the weight of woollen sweater, leaves standstill 420min at being then placed in 35 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Embodiment 2:
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1.5*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.0%, pigskin collagen 0.9%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 25 DEG C puts 15 hours, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.05 times of the weight of woollen sweater, leaves standstill 350min at being then placed in 39 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Embodiment 3:
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1.1*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.4%, pigskin collagen 0.7%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 27 DEG C puts 13 hours, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.07 times of the weight of woollen sweater, leaves standstill 400min at being then placed in 36 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Embodiment 4:
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1.4*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.2%, pigskin collagen 0.8%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 26 DEG C puts 14 hours, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.06 times of the weight of woollen sweater, leaves standstill 370min at being then placed in 38 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Embodiment 5 contrast test:
In the present invention, the collocation of preliminary treatment and microbial inoculum is all extremely important, if the ratio of not carrying out preliminary treatment or microbial inoculum is not right, all can have a strong impact on effect, infers and serves certain synergy between each parameter.
Comparative example 1: carry out preliminary treatment without A agent
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1.3*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
(2) arrange:
A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.07 times of the weight of woollen sweater, leaves standstill 410min at being then placed in 37 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Comparative example 2: the ratio of bacterial strain is not right
The application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:1:1 is mixed with 1.2*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.3%, pigskin collagen 0.6%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 25 DEG C puts 15 hours, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.08 times of the weight of woollen sweater, leaves standstill 390min at being then placed in 35 DEG C, dries in the process of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
Embodiment 6: index is tested and assessed
The index of the woollen sweater that embodiment 1-5 obtains is tested, as follows:
Wool weight-loss ratio measures:
According to fabric regain, calculate the treated front constant dry mass w0 of sample; The constant dry mass w1 of fabric after precise process, is calculated as follows the weight-loss ratio before and after fabric ferment treatment:
Weight-loss ratio=(w0-w1)/w0 × 100%
The pilling resistance of tricot de laine detects and adopts GB/T4802.3-2008 balling-up case method.
Evaluate the persistence of antibacterial fabric performance, mainly antibiotic fabric is carried out to the wash durability test of anti-microbial property.Antibiotic fabric decantation test with reference to the simplification wash conditions of appendix C in " FZ/T73023-2006 antibiosis knitting product " and program, to fabric washing to be measured 50 times.
Antibiotic fabric performance test methods is with reference to the succusion of Appendix D in " FZ/T73023-2006 antibiosis knitting product ".Succusion be imitate human body wear condition, make bacterium under oscillating condition with anti-microbial agent in clothes, by calculate bacterial reduction, determine a kind of method of anti-microbial property size.Succusion testing procedure is: put into by sample to be tested containing certain density bacterium (staphylococcus aureus bacterial classification) nutrient solution, then sample is placed on reciprocating oscillator, at (24 ± 1) DEG C, with the velocity fluctuation 18h of 150r/min, sample fabric is fully contacted by vibration with bacterium liquid after, 24h is cultivated in (37 ± 1) DEG C biochemical cultivation case, measure the clump count of bacterium before and after vibration, carry out quantitative assessment antibacterial effect by method for counting colonies.
The calculating of succusion test anti-microbial property:
Bacteriostasis rate (%)=(A-B)/A × 100%
In formula (1): A is clump count after standard blank sample vibration 18h; B is clump count after sample to be tested vibration 18h.
Table 1 detects for producing to embodiment 1-5 the woollen sweater obtained the result obtained.
Table 1 performance measurement
This detects data only for above-mentioned detection sample.
As can be seen here, the invention provides the application of a kind of ecological auxiliary agent on woollen sweater arranges, described ecological auxiliary agent comprises compound live bacteria agent, native protein, natural polysaccharides etc., not containing any chemical reagent, use simple, woollen sweater after arrangement has good antibacterial effect, and can also ANTIPILLING, makes the feel of woollen sweater finer and smoother, there is gloss. in addition, the mechanical strength also observing woollen sweater after arranging strengthens, upper dye, on whiteness then without any impact.
The above; be only the present invention's preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (2)
1. the application of ecological auxiliary agent on woollen sweater arranges, its step is as follows:
(1) ecological auxiliary agent is prepared:
A agent: will addicted to sour micrococcus, bacillus subtilis, Candida is that 1:0.3:0.5 is mixed with 1-1.5*10 according to bacterial strain number ratio
5bacteria suspension, described bacteria suspension also contains, according to mass percent, the trehalose of 0.3%, the stachyose of 0.2%, the nano titanium oxide of 0.05%;
B agent: according to mass percent, fibroin albumen 1.0-1.5%, pigskin collagen 0.6=0.9%, water soluble chitosan 0.2%, 0.08% nano titanium oxide;
(2) arrange:
First B agent be evenly sprayed on woollen sweater, the weight of sprinkling is 0.1 times of the weight of woollen sweater, vexedly at being then placed in 25-28 DEG C puts 12-15 hour, 30 DEG C of oven dry, for subsequent use;
Then A agent be evenly sprayed on the woollen sweater of oven dry, the weight of sprinkling is 0.05-0.08 times of the weight of woollen sweater, leaves standstill 350-420min at being then placed in 35-39 DEG C, dries in the processes of leaving standstill for 30 DEG C and keeps constant temperature and ventilation;
(3) with washed with de-ionized water fabric face residue, 60 DEG C cure 5s after, 30 DEG C of oven dry.
2. the application of ecological auxiliary agent according to claim 1 on woollen sweater arranges, is characterized in that:
The molecular weight of described nano titanium oxide is 50-100nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510770772.8A CN105256568A (en) | 2015-11-12 | 2015-11-12 | Application of ecological auxiliary to woolen sweater finishing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510770772.8A CN105256568A (en) | 2015-11-12 | 2015-11-12 | Application of ecological auxiliary to woolen sweater finishing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105256568A true CN105256568A (en) | 2016-01-20 |
Family
ID=55096484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510770772.8A Pending CN105256568A (en) | 2015-11-12 | 2015-11-12 | Application of ecological auxiliary to woolen sweater finishing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105256568A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106223002A (en) * | 2016-07-27 | 2016-12-14 | 罗敏凯 | A kind of automotive trim is with high-grade sun-resistant wool fabric |
| CN106223042A (en) * | 2016-07-27 | 2016-12-14 | 罗敏凯 | A kind of automotive trim Pilus Caprae seu Ovis aloe fibre blend fabric |
| CN106245309A (en) * | 2016-07-27 | 2016-12-21 | 罗敏凯 | A kind of soybean fiber blended fabric of automotive trim Pilus Caprae seu Ovis |
| CN109797546A (en) * | 2019-01-22 | 2019-05-24 | 乐清市雅格狮丹服饰有限公司 | A kind of warm-keeping overcoat finishing technique |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677465A (en) * | 2012-05-23 | 2012-09-19 | 辽东学院 | Modified tussah silk fabric with functionalized nanometer chitosan and nanometer titanium dioxide |
| CN103266480A (en) * | 2013-06-13 | 2013-08-28 | 太仓协大申泰羊毛衫有限公司 | Method for preventing wool from fluffing and pilling |
| CN104594029A (en) * | 2015-02-02 | 2015-05-06 | 苏州爱立方服饰有限公司 | Antibacterial finish method for blended cotton fabric |
| CN105031711A (en) * | 2015-06-17 | 2015-11-11 | 郑州大学 | Collagen/chitosan composite sponge biological dressing and preparation method thereof |
-
2015
- 2015-11-12 CN CN201510770772.8A patent/CN105256568A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677465A (en) * | 2012-05-23 | 2012-09-19 | 辽东学院 | Modified tussah silk fabric with functionalized nanometer chitosan and nanometer titanium dioxide |
| CN103266480A (en) * | 2013-06-13 | 2013-08-28 | 太仓协大申泰羊毛衫有限公司 | Method for preventing wool from fluffing and pilling |
| CN104594029A (en) * | 2015-02-02 | 2015-05-06 | 苏州爱立方服饰有限公司 | Antibacterial finish method for blended cotton fabric |
| CN105031711A (en) * | 2015-06-17 | 2015-11-11 | 郑州大学 | Collagen/chitosan composite sponge biological dressing and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 孔令杰 等: "羊毛抗菌整理研究进展", 《纺织导报》 * |
| 陈韶娟 马建伟: "纳米二氧化钛复合抗菌剂的抗菌性及抗菌原理", 《第五届功能性纺织品及纳米技术研讨会论文集》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106223002A (en) * | 2016-07-27 | 2016-12-14 | 罗敏凯 | A kind of automotive trim is with high-grade sun-resistant wool fabric |
| CN106223042A (en) * | 2016-07-27 | 2016-12-14 | 罗敏凯 | A kind of automotive trim Pilus Caprae seu Ovis aloe fibre blend fabric |
| CN106245309A (en) * | 2016-07-27 | 2016-12-21 | 罗敏凯 | A kind of soybean fiber blended fabric of automotive trim Pilus Caprae seu Ovis |
| CN109797546A (en) * | 2019-01-22 | 2019-05-24 | 乐清市雅格狮丹服饰有限公司 | A kind of warm-keeping overcoat finishing technique |
| CN109797546B (en) * | 2019-01-22 | 2021-04-27 | 乐清市雅格狮丹服饰有限公司 | Finishing process of warm overcoat |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105239413A (en) | Application of ecological auxiliary in finishing of cashmere sweater | |
| CN105455263B (en) | A kind of antibacterial woollen sweater of anti pilling | |
| CN105421055A (en) | Moisture-absorbing and perspiring anti-bacterial fabric and preparation technology thereof | |
| CN105256568A (en) | Application of ecological auxiliary to woolen sweater finishing | |
| CN105625032A (en) | Ultraviolet-proof polyester-cotton fabric and preparation method thereof | |
| CN105420890A (en) | Cool and antibacterial shell fabric and preparation process thereof | |
| CN104294595A (en) | Production process for anti-bacterial deodorant textile | |
| CN111304918B (en) | Antibacterial fabric and preparation method thereof | |
| CN105256590A (en) | Ecological textile auxiliary | |
| CN105088460A (en) | Textile material and preparation method thereof | |
| CN105200775A (en) | Antibacterial soft finishing process of dacron fabric | |
| CN105077783A (en) | Skincare aromatic textile material and preparation method thereof | |
| CN109468844A (en) | Antibacterial fabric and its production technology | |
| CN109457466A (en) | Functionalized carbon nano-tube and its application in antistatic antibiotic fabric finishing liquor | |
| CN105780233A (en) | Textile material and manufacture method thereof | |
| CN107237017A (en) | A kind of textile material and preparation method thereof | |
| CN105220483A (en) | A kind of antibacterial finish technique of cashmere sweater | |
| CN105908307A (en) | Textile material and preparation method thereof | |
| CN105908308A (en) | Textile material and preparation method thereof | |
| CN105133141A (en) | Skin-caring fragrant textile material and preparing method thereof | |
| CN105220459A (en) | A kind of antibiotic soft finishing auxiliaries of polyester fabric | |
| CN105256570A (en) | Finishing auxiliary of woolen sweater | |
| CN105220491A (en) | A kind of antibacterial finish technique of woollen sweater | |
| CN1093188C (en) | Bacteriostatic odour-resistant blended yarn, its preparation method and application | |
| CN105442318A (en) | Sun-protecting and antibacterial finishing auxiliary agent for cashmere sweaters |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160120 |
|
| RJ01 | Rejection of invention patent application after publication |