CN114591699A - Preparation method of binder for textiles - Google Patents
Preparation method of binder for textiles Download PDFInfo
- Publication number
- CN114591699A CN114591699A CN202110499993.1A CN202110499993A CN114591699A CN 114591699 A CN114591699 A CN 114591699A CN 202110499993 A CN202110499993 A CN 202110499993A CN 114591699 A CN114591699 A CN 114591699A
- Authority
- CN
- China
- Prior art keywords
- stirring
- polyethylene
- coupling agent
- silane coupling
- vinyl alcohol
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a binder for textiles, which comprises the steps of adding superfine silicon dioxide into polyethylene glycol, heating to 75-80 ℃, stirring for 25-40 min, adding polydopamine, keeping the temperature, continuously stirring for 20-30 min, moving into a microwave oven, drying at 80-85 ℃, and grinding through a 800-1000 mesh screen to obtain modified nano silicon dioxide; adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 40-60 min at 80-85 ℃, adding guar gum into the container, stirring and dissolving, then stirring and reacting at 60-65 ℃ under the protection of nitrogen, dropwise adding hydrogen peroxide in the stirring process, finishing dropwise adding within 30min, and adding the modified nano silicon dioxide and the silane coupling agent in the step S1 to continuously react for 20-30 min after dropwise adding; and (5) continuously adding sodium dodecyl sulfate into the step S2, heating to 80-90 ℃, stirring for reacting for 40-60 min, and cooling to obtain the binder.
Description
Technical Field
The invention belongs to the technical field of textiles, and particularly relates to a preparation method of a binder for textiles.
Background
The textile fabric is a flat flexible sheet-shaped object formed by fine flexible objects through crossing, winding or bonding. The plurality of yarns are in a stable relationship to form the fabric. Crossovers and kinks are two stable structural relationships that yarns can make up. The fabric keeps stable shape and specific mechanical property. Various fabrics can be clearly known by analyzing the yarn groups in the fabrics and the running direction, the running rule and the formed relationship thereof. The existing cloth has a plurality of varieties, but along with the continuous improvement of the living standard of people, the existing cloth has single performance, and a new variety capable of meeting the requirements of different crowds needs to be provided.
The binder is a guarantee of the bonding strength between the abrasive and the matrix. With the development of the chemical industry, various novel binders enter the field of coated abrasives, the performance of the coated abrasives is improved, and the development of the coated abrasive industry is promoted. Besides the sizing material, the adhesive also comprises auxiliary components such as a solvent, a curing agent, a toughening agent, a preservative, a coloring agent, a defoaming agent and the like. Binders include synthetic resins, rubbers and paints in addition to the most commonly used animal glues. The prior adhesive is hard after being dried, so that an obvious boundary layer is formed between different melamine foam adhesive layers, and the adhesive has poor hand feeling when in use; moreover, harmful substances can volatilize to pollute the air in the production process of the conventional adhesive, and the production process has the disadvantages of long time consumption, high energy consumption and energy waste.
Disclosure of Invention
The invention aims to provide a preparation method of a textile binder, which comprises the following steps:
s1: adding superfine silicon dioxide into polyethylene glycol, heating to 75-80 ℃, stirring for 25-40 min, adding polydopamine, keeping the temperature, continuously stirring for 20-30 min, transferring into a microwave oven, drying at 80-85 ℃, and grinding through a 800-1000 mesh screen to obtain the modified nano silicon dioxide, wherein the mass ratio of the polyethylene-vinyl alcohol to the polydopamine is (1-1.6) to (1.05-1.86).
S2: adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 40-60 min at 80-85 ℃, adding guar gum into the container, stirring and dissolving, then stirring and reacting at 60-65 ℃ under the protection of nitrogen, dropwise adding hydrogen peroxide in the stirring process, completing dropwise adding within 30min, and adding the modified nano silicon dioxide and the silane coupling agent in the step S1 to continuously react for 20-30 min after completing dropwise adding.
S3: and (2) continuously adding sodium dodecyl sulfate into the step (S2), heating to 80-90 ℃, stirring for reacting for 40-60 min, and cooling to obtain the binder, wherein the mass ratio of the sodium dodecyl sulfate to the polyethylene-vinyl alcohol is (0.2-0.5): (0.84-2.88).
Preferably, the mass fraction of the hydrogen peroxide relative to the polyethylene-vinyl alcohol is 6 to 10%; the mass ratio of the added hydrogen peroxide to the polyethylene-vinyl alcohol is (2.2-3.4) to (1-1.65).
Preferably, the mass ratio of the polyethylene-vinyl alcohol, the water, the guar gum, the modified nano-silica in the step S1 and the silane coupling agent is (1.6-2.4): (5-10): (0.7-1.1): (0.8-1.35): 0.65-1.05).
Preferably, the silane coupling agent is any one of a silane coupling agent HK550, a silane coupling agent HK570, a silane coupling agent HK560, a silane coupling agent HK-590 or a silane coupling agent A-172.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, polyethylene glycol and polydopamine are used for modifying nano silicon dioxide, polyethylene-vinyl alcohol (EVOH) and water are added into a container, then stirring and reacting for 40-60 min at the temperature of 80-85 ℃, then adding the guar gum into a container, stirring and dissolving, then stirring and reacting under the protection of nitrogen and controlling the temperature to be 60-65 ℃, dropwise adding hydrogen peroxide in the stirring process, finishing dropwise adding within 30min, adding the modified nano-silica and the silane coupling agent after finishing dropwise adding, continuously reacting for 20-30 min, continuously adding sodium dodecyl sulfate, heating to 80-90 ℃, stirring and reacting for 40-60 min, cooling to obtain a binder, the adhesive has moderate viscosity and pH value, small change of stripping strength before and after washing, and simultaneously after the fabric is treated, the breaking strength and the air permeability of the fabric are changed slightly, and the adhesive provided by the invention has excellent air permeability and toughness while playing a role in bonding the fabric.
Detailed Description
The following detailed description of the embodiments of the present invention is provided for the purpose of illustration, and the detailed implementation and specific operation procedures are given, it should be noted that those skilled in the art can make various modifications and amendments without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Example 1
The preparation method of the textile adhesive specifically comprises the following steps:
s1: adding superfine silicon dioxide into polyethylene glycol, heating to 75 ℃, stirring for 25min, adding polydopamine, keeping the temperature, continuously stirring for 20min, moving to a microwave oven, drying at 80 ℃, and grinding through a 800-mesh screen to obtain the modified nano silicon dioxide, wherein the mass ratio of the polyethylene-vinyl alcohol to the polydopamine is 1: 1.05.
S2: adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 40min at 80 ℃, then adding guar gum into the container, stirring and dissolving, then stirring and reacting under the protection of nitrogen and at 60 ℃, dropwise adding 6% of hydrogen peroxide relative to the mass fraction of the polyethylene-vinyl alcohol during stirring, and finishing dropwise adding within 30min, wherein the mass ratio of the hydrogen peroxide to the polyethylene-vinyl alcohol is 2.2:1, and after dropwise adding, adding the modified nano silicon dioxide in the step S1 and the silane coupling agent HK560 to continue reacting for 20min, wherein the mass ratio of the polyethylene-vinyl alcohol to the water to the guar gum to the modified nano silicon dioxide in the step S1 and the silane coupling agent HK560 is 1.6:5:0.7:0.8: 0.65.
S3: and (3) continuously adding sodium dodecyl sulfate into the step S2, heating to 80 ℃, stirring for reacting for 40min, and cooling to obtain the binder, wherein the mass ratio of the sodium dodecyl sulfate to the polyethylene-vinyl alcohol is 0.2: 0.84.
example 2
The preparation method of the textile adhesive specifically comprises the following steps:
s1: adding the superfine silicon dioxide into polyethylene glycol, heating to 80 ℃, stirring for 40min, adding polydopamine, keeping the temperature, continuously stirring for 30min, transferring to a microwave oven, drying at 85 ℃, and grinding through a 1000-mesh screen to obtain the modified nano-silicon dioxide, wherein the mass ratio of the polyethylene-vinyl alcohol to the polydopamine is 1.6: 1.86.
S2: adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 60min at 80-85 ℃, adding guar gum into the container, stirring and dissolving, then stirring and reacting at 65 ℃ under the protection of nitrogen, dropwise adding hydrogen peroxide accounting for 10% of the mass fraction of the polyethylene-vinyl alcohol in the stirring process, and dropwise adding the hydrogen peroxide within 30min, wherein the mass ratio of the hydrogen peroxide to the polyethylene-vinyl alcohol is 3.4:1.65, adding the modified nano silicon dioxide in the step S1 and a silane coupling agent HK-590 after dropwise adding, and continuing reacting for 30min, wherein the mass ratio of the polyethylene-vinyl alcohol, the water, the guar gum, the modified nano silicon dioxide in the step S1 and the silane coupling agent HK-590 is 2.4:10:1.1:1.35: 1.05.
S3: and (3) continuously adding sodium dodecyl sulfate into the step S2, heating to 90 ℃, stirring and reacting for 60min, and cooling to obtain the binder, wherein the mass ratio of the sodium dodecyl sulfate to the polyethylene-vinyl alcohol is 0.5: 2.88.
example 3
A preparation method of a textile adhesive specifically comprises the following steps:
s1: adding superfine silicon dioxide into polyethylene glycol, heating to 78 ℃, stirring for 30min, adding polydopamine, keeping the temperature, continuously stirring for 25min, moving to a microwave oven, drying at 82 ℃, and grinding through a 900-mesh screen to obtain the modified nano silicon dioxide, wherein the mass ratio of the polyethylene-vinyl alcohol to the polydopamine is 1.4: 1.62.
S2: adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 50min at 82 ℃, adding guar gum into the container, stirring and dissolving, then stirring and reacting at 62 ℃ under the protection of nitrogen, dropwise adding 8% of hydrogen peroxide relative to the mass fraction of the polyethylene-vinyl alcohol during stirring, and finishing dropwise adding within 30min, wherein the mass ratio of the hydrogen peroxide to the polyethylene-vinyl alcohol is 2.9:1.54, and after dropwise adding, adding the modified nano-silica in the step S1 and the silane coupling agent A-172 to continue reacting for 25min, wherein the mass ratio of the polyethylene-vinyl alcohol to the water to the guar gum to the modified nano-silica in the step S1 and the silane coupling agent A-172 is 2.1:8:0.9:1.28: 0.96.
S3: and (2) continuously adding sodium dodecyl sulfate into the step S2, heating to 85 ℃, stirring and reacting for 50min, and cooling to obtain the binder, wherein the mass ratio of the sodium dodecyl sulfate to the polyethylene-vinyl alcohol is 0.35: 1.58.
examples of the experiments
Performance test 1-the adhesive prepared in example 1-3 is placed in an oven at 25 ℃ for storage, and after being stabilized for 12 hours, the viscosity of the adhesive is tested by selecting a 27-rotor with the rotation speed of 60rpm according to a standard GB/T2794-1995 in testing an SNB-3 digital viscometer; measuring the pH value of the solution by using a pH meter; the water resistance test is to place the binder prepared in the embodiment 1-3 into an SWB-12 type A washing fastness instrument, wherein the bath ratio is about 50:1, the dosage of the detergent is 2g/L, the water temperature is 40 ℃, the washing time is 45min, then the binder is naturally dried, and the stripping strength after washing is tested; the adhesive prepared in examples 1-3 was tested by peeling strength according to standard GB/T2791-1995 and a material tester for a sample of 200mm × 25mm,
table 1. test results:
as can be seen from table 1, the binders prepared in examples 1 to 3 of the present invention all had a viscosity of about 2015mpa.s, and also had excellent properties in terms of peel strength and peel strength after washing with water.
Performance test 2-the binder prepared in examples 1-3 was used in a fabric, and the fabric was then subjected to a warp-wise treatment according to GB/T3923.1-2013 "first part of tensile properties of textile fabrics: a determination strip sample method of breaking strength and breaking elongation, namely performing breaking strength test on a fabric by adopting an Instron 5967 type universal material testing machine, and taking an average value of 3 times of measurement; the air permeability of the fabric was measured according to GB/T5453-1997 method for measuring air permeability of fabric, with a test pressure difference of 100Pa, and 3 measurements were taken for each sample, the test results are shown in Table 2,
table 2. test results:
as can be seen from Table 2, the breaking strength of the original cloth of the adhesive prepared in the embodiments 1 to 3 of the present invention is above 1008.47N, and the air permeability is 152.26L (m)2·s)-1As described above, the binder of the present invention does not cause damage to the breaking strength and air permeability of the original cloth.
Claims (4)
1. The preparation method of the textile adhesive is characterized by comprising the following steps:
s1: adding superfine silicon dioxide into polyethylene glycol, heating to 75-80 ℃, stirring for 25-40 min, adding polydopamine, keeping the temperature, continuously stirring for 20-30 min, then moving into a microwave oven, drying at 80-85 ℃, and then grinding through a 800-1000 mesh screen to obtain modified nano silicon dioxide, wherein the mass ratio of polyethylene-vinyl alcohol to polydopamine is (1-1.6) to (1.05-1.86);
s2: adding polyethylene-vinyl alcohol (EVOH) and water into a container, stirring and reacting for 40-60 min at 80-85 ℃, adding guar gum into the container, stirring and dissolving, then stirring and reacting at 60-65 ℃ under the protection of nitrogen, dropwise adding hydrogen peroxide in the stirring process, finishing dropwise adding within 30min, and adding the modified nano silicon dioxide and the silane coupling agent in the step S1 to continuously react for 20-30 min after dropwise adding;
s3: and (2) continuously adding sodium dodecyl sulfate into the step (S2), heating to 80-90 ℃, stirring for reacting for 40-60 min, and cooling to obtain the binder, wherein the mass ratio of the sodium dodecyl sulfate to the polyethylene-vinyl alcohol is (0.2-0.5): (0.84-2.88).
2. The preparation method of the textile binder according to claim 1, wherein the mass fraction of the hydrogen peroxide relative to the polyethylene-vinyl alcohol is 6-10%; the mass ratio of the added hydrogen peroxide to the polyethylene-vinyl alcohol is (2.2-3.4) to (1-1.65).
3. The method for preparing a textile binder as defined in claim 1, wherein the mass ratio of the polyethylene-vinyl alcohol, the water, the guar gum, the modified nano silica in step S1 and the silane coupling agent is (1.6-2.4): 5-10): 0.7-1.1): 0.8-1.35): 0.65-1.05.
4. The method for preparing a binder for textiles as claimed in claim 1, wherein the silane coupling agent is any one of silane coupling agent HK550, silane coupling agent HK570, silane coupling agent HK560, silane coupling agent HK-590 or silane coupling agent A-172.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110499993.1A CN114591699A (en) | 2021-05-08 | 2021-05-08 | Preparation method of binder for textiles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110499993.1A CN114591699A (en) | 2021-05-08 | 2021-05-08 | Preparation method of binder for textiles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114591699A true CN114591699A (en) | 2022-06-07 |
Family
ID=81803770
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110499993.1A Pending CN114591699A (en) | 2021-05-08 | 2021-05-08 | Preparation method of binder for textiles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114591699A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114891370A (en) * | 2022-06-15 | 2022-08-12 | 张木彬 | Coated anatase titanium dioxide and preparation method thereof |
| CN116874233A (en) * | 2023-07-04 | 2023-10-13 | 清远楼邦建材科技有限公司 | Mortar adhesive composition and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327793A (en) * | 2014-08-06 | 2015-02-04 | 桐乡嘉力丰实业股份有限公司 | Inorganic-powder-modified mould-proof wallpaper adhesive and preparation method thereof |
| CN109957336A (en) * | 2017-12-25 | 2019-07-02 | 中国科学院上海硅酸盐研究所 | A kind of haze-proof mask binder and preparation method thereof |
| GB202103994D0 (en) * | 2021-03-23 | 2021-05-05 | Zhuang wuyi | A preparation method of binder for textile |
-
2021
- 2021-05-08 CN CN202110499993.1A patent/CN114591699A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327793A (en) * | 2014-08-06 | 2015-02-04 | 桐乡嘉力丰实业股份有限公司 | Inorganic-powder-modified mould-proof wallpaper adhesive and preparation method thereof |
| CN109957336A (en) * | 2017-12-25 | 2019-07-02 | 中国科学院上海硅酸盐研究所 | A kind of haze-proof mask binder and preparation method thereof |
| GB202103994D0 (en) * | 2021-03-23 | 2021-05-05 | Zhuang wuyi | A preparation method of binder for textile |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114891370A (en) * | 2022-06-15 | 2022-08-12 | 张木彬 | Coated anatase titanium dioxide and preparation method thereof |
| CN114891370B (en) * | 2022-06-15 | 2023-09-22 | 衡水澳德彩建筑装饰材料有限公司 | Coated anatase titanium dioxide and preparation method thereof |
| CN116874233A (en) * | 2023-07-04 | 2023-10-13 | 清远楼邦建材科技有限公司 | Mortar adhesive composition and preparation method thereof |
| CN116874233B (en) * | 2023-07-04 | 2024-02-06 | 清远楼邦建材科技有限公司 | Mortar adhesive composition and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114591699A (en) | Preparation method of binder for textiles | |
| CN103141975B (en) | A kind of production technology of bamboo fibre double-point lining cloth | |
| WO2018099150A1 (en) | Aqueous double-sided-suede microfiber pu synthetic leather and preparation method therefor | |
| CN105155297B (en) | A kind of preparation method of aqueous polyurethane impregnation superfine fiber chemical leather bass | |
| CN106521986A (en) | Aqueous double-faced suede microfiber PU synthetic leather and production method thereof | |
| CN103126140B (en) | Production process of cashmere lining cloth | |
| CN105667061B (en) | A kind of production technology of sofa fabric | |
| CN105671989A (en) | Soft sheepskin-imitating polyurethane resin, preparation method thereof, and method of producing sheepskin-imitating artificial leather therewith | |
| CN106256941A (en) | A kind of base fabric production technology for coated fabric and application thereof | |
| CN109501426A (en) | The production method of 3D solid vertical bar bubble wrinkle latitude elasticity fabric | |
| CN112301505A (en) | Seamless down-filled down jacket fabric and production method thereof | |
| GB2590037A (en) | A preparation method of binder for textile | |
| CN106638020A (en) | Composite functional lace fabric dyeing and finishing method | |
| CN110527465B (en) | Flocking adhesive for spinning and preparation method thereof | |
| CN111890756A (en) | Ageing-resistant gold stamping process for decorative fabric | |
| CN109914118B (en) | Three proofings fly to knit vamp | |
| CN113622201B (en) | Polyurethane synthetic leather with high moisture absorption and air permeability and preparation method thereof | |
| CN105644125B (en) | A kind of preparation method of suede nap composite polyurethane sofa cloth | |
| CN111286852A (en) | Preparation method of long-acting anti-fouling fabric based on nanogel treatment | |
| CN112064169A (en) | Crease-resistant breathable suit fabric | |
| CN109972332A (en) | Wash water carrier and washing method | |
| CN105239426A (en) | Washable lightfast clothes dye | |
| CN111647128B (en) | Preparation method of formaldehyde-free textile color fixing agent | |
| CN109371659B (en) | Preparation method of heavy silk fabric based on digital printing | |
| KR101712983B1 (en) | Eco friendly vintage dyeing process for Fabric and Fabric prepared therefrom |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |