CN112868650A - Bactericide and preparation method and application thereof - Google Patents
Bactericide and preparation method and application thereof Download PDFInfo
- Publication number
- CN112868650A CN112868650A CN202110152290.1A CN202110152290A CN112868650A CN 112868650 A CN112868650 A CN 112868650A CN 202110152290 A CN202110152290 A CN 202110152290A CN 112868650 A CN112868650 A CN 112868650A
- Authority
- CN
- China
- Prior art keywords
- compound
- bactericide
- polymer
- water
- 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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
- A01N33/20—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/34—Nitriles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
Abstract
The invention discloses a bactericide and a preparation method and application thereof, and the bactericide at least comprises the following components: alcohol polymer, aliphatic nitro compound, amido bond compound and halogenated compound. The components are put into a reaction kettle, and the product is obtained after uniform stirring and mixing. The bactericide prepared by the invention has the advantages of simple production process, high economic benefit and excellent bactericidal effect, can be retained in a water system for a long time, and ensures the continuous bactericidal effect of the bactericide. The bactericide prepared by the invention is widely used for sterilization in the water treatment process, and at least comprises the steps of wastewater treatment, water purification treatment, reclaimed water recycling, seawater desalination, agricultural products, leather products, furniture products, animal husbandry and aquaculture.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a bactericide and a preparation method and application thereof.
Technical Field
Biocides, also known as biocides, bactericidal algicides, microbicides, and the like, generally refer to chemical agents that are effective in inhibiting or killing microorganisms in aqueous systems.
Currently used bactericides can be divided into two main categories, namely oxidizing bactericides and non-oxidizing bactericides. Industrial fungicides are used to kill bacteria, viruses and algae. The common industrial oxidizing bactericide is a chlorine-containing compound, peroxide, a bromine-containing compound and the like, and has the advantages of high speed of sterilizing and algae killing, high broad spectrum of biocidal effect, small relative influence on environmental pollution and difficult generation of drug resistance of microorganisms, for example, the bactericide containing 2, 2-dibromo-3-nitrilopropionamide can quickly kill bacteria in water, the reaction is usually completed within 1 hour, but the oxidizing bactericide is easily influenced by organic matters and reducing substances in water, the decomposition speed of the bactericide is high, the bactericide cannot be retained for a long time, the volatilization of the bactericidal efficacy of the bactericide is influenced, and the bactericidal effect cannot reach the expected purpose.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a bactericide.
A fungicide, comprising at least: alcohol polymer, aliphatic nitro compound, amido bond compound and halogenated compound.
Further, the bactericide comprises the following components in percentage by weight: 1-50% of alcohol polymer; 1-20% of aliphatic nitro compound; amide bond compound 0.1-5%; 0.1-5% of halogenated compound; and supplementing the balance of water.
Further, the bactericide comprises the following components in percentage by weight: 45-50% of alcohol polymer; 15-20% of aliphatic nitro compound; 0.1-3% of amido bond compound; 0.1-2% of halogenated compound; and supplementing the balance of water.
Further, the bactericide comprises the following components in percentage by weight: 45-50% of alcohol polymer; 15-20% of aliphatic nitro compound; 0.1-1% of amido bond compound; 0.1-1% of halogenated compound; and supplementing the balance of water.
Further, the alcohol polymer is at least one of a monohydric alcohol polymer, a dihydric alcohol polymer, a trihydric alcohol polymer and a polyhydric alcohol polymer.
Further, the glycol polymer is at least one selected from the group consisting of PEG200, PEG400, and PEG 600.
Further, the aliphatic nitro compound is at least one selected from 2-bromo-2-nitro-1, 3-propanediol and 2, 2-dibromo-2-nitroethanol.
Further, the amide bond compound is at least one selected from the group consisting of 2, 2-dibromo-3-nitrilopropionamide and 2, 2-dibromomalonamide.
Further, the halogenated compound is at least one selected from ammonium bromide, bromoacetonitrile, potassium iodide, sodium hypochlorite and dichlorohydantoin.
In a second aspect, the invention provides a method for preparing a bactericide.
A method for preparing a bactericide comprises the following steps: the components are sequentially put into a reaction kettle, and the product is obtained after uniform stirring and mixing.
The third aspect of the invention provides the application field of the bactericide.
The application field of the bactericide at least comprises the following steps: wastewater treatment, water purification, reclaimed water recycling, seawater desalination, agricultural products, leather products, furniture products, animal husbandry and aquaculture.
Compared with the prior art, the invention has the beneficial effects that:
1. the bactericide prepared by the invention can be widely applied to sterilization in the water treatment process, and the bactericide developed by the invention has the advantages of simple production process, low cost, suitability for large-scale production, high economic benefit, excellent sterilization effect and high sterilization rate up to 99.5%;
2. the bactericide prepared by the invention can be remained in a water system for a long time, and further plays a synergistic action under the condition of the ingredients of the active ingredients, so that the stability of the bactericide is improved, and the continuous sterilizing effect of the bactericide is ensured.
Detailed Description
In order to solve the above problems, the present invention provides a bactericide.
A fungicide, comprising at least: alcohol polymer, aliphatic nitro compound, amido bond compound and halogenated compound.
Further, the bactericide comprises the following components in percentage by weight: 1-50% of alcohol polymer; 1-20% of aliphatic nitro compound; amide bond compound 0.1-5%; 0.1-5% of halogenated compound; and supplementing the balance of water.
Further, the bactericide comprises the following components in percentage by weight: 45-50% of alcohol polymer; 15-20% of aliphatic nitro compound; 0.1-3% of amido bond compound; 0.1-2% of halogenated compound; and supplementing the balance of water.
Further, the bactericide comprises the following components in percentage by weight: 45-50% of alcohol polymer; 15-20% of aliphatic nitro compound; 0.1-1% of amido bond compound; 0.1-1% of halogenated compound; and supplementing the balance of water.
Further, the alcohol polymer is at least one of a monohydric alcohol polymer, a dihydric alcohol polymer, a trihydric alcohol polymer and a polyhydric alcohol polymer.
Further, the glycol polymer is at least one selected from the group consisting of PEG200, PEG400, and PEG 600.
Further, the aliphatic nitro compound is at least one selected from 2-bromo-2-nitro-1, 3-propanediol and 2, 2-dibromo-2-nitroethanol.
Further, the amide bond compound is at least one selected from the group consisting of 2, 2-dibromo-3-nitrilopropionamide and 2, 2-dibromomalonamide.
Further, the halogenated compound is at least one selected from ammonium bromide, bromoacetonitrile, potassium iodide, sodium hypochlorite and dichlorohydantoin.
Further, the aliphatic nitro compound is 2-bromo-2-nitro-1, 3-propanediol.
The aliphatic nitro compound is hardly soluble in water and is easily decomposed in an alkaline solution.
The molecular structure of the 2-bromo-2-nitro-1, 3-propanediol is as follows:
further, the amido bond compound is 2, 2-dibromo-3-nitrilopropionamide.
The amide bond compound refers to a compound obtained by substituting hydrogen on a nitrogen atom of ammonia or amine with an acyl group, and can also be regarded as a derivative of ammonia or amine.
The molecular structure of the 2, 2-dibromo-3-nitrilopropionamide is as follows:
the halogenated compound is a compound in which a functional group in an organic compound is substituted with a halogen element, and a halogen ion is easily dissociated from the halogenated compound.
The 2-bromine-2-nitro-1, 3-propylene glycol is easy to decompose under the alkaline condition and loses the sterilization effect, the bactericide system of the invention contains nitro and amino, and simultaneously, the ammonium bromide and PEG200 contained in the bactericide system of the invention generate excellent synergistic effect with other raw materials in the system, thereby relieving the decomposition of the 2-bromine-2-nitro-1, 3-propylene glycol, improving the stability of the bactericide and ensuring the continuous sterilization effect.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
PEG200 was purchased from kay chemical ltd, shanghai, CAS No.: 25322-68-3.
2-bromo-2-nitro-1, 3-propanediol was purchased from south kyoto biotechnology limited, CAS No.: 52-51-7.
2, 2-dibromo-3-nitrilopropionamide was purchased from taikupu source pharmaceutical raw materials ltd, CAS no: 10222-01-2.
Ammonium bromide was purchased from bailing technologies ltd, beijing, CAS no: 12124-97-9.
Example 1
A bactericide comprises the following components in percentage by weight: PEG 20045%; 15% of 2-bromo-2-nitro-1, 3-propanediol; 1% of 2, 2-dibromo-3-nitrilopropionamide; 1% of ammonium bromide; and supplementing the balance of water.
The components are sequentially put into a reaction kettle, and are stirred and mixed uniformly to obtain a bactericide product 1.
Example 2
A bactericide comprises the following components in percentage by weight: PEG 20050%; 20% of 2-bromo-2-nitro-1, 3-propanediol; 1% of 2, 2-dibromo-3-nitrilopropionamide; 1% of ammonium bromide; and supplementing the balance of water.
And (3) sequentially putting the components into a reaction kettle, and uniformly stirring and mixing to obtain a bactericide product 2.
Example 3
A bactericide comprises the following components in percentage by weight: PEG 20050%; 20% of 2-bromo-2-nitro-1, 3-propanediol; 0.1 percent of 2, 2-dibromo-3-nitrilopropionamide; 0.1% of ammonium bromide; and supplementing the balance of water.
And (3) sequentially putting the components into a reaction kettle, and uniformly stirring and mixing to obtain a bactericide product 3.
Comparative example 1
A bactericide comprises the following components in percentage by weight: PEG 20048%; 15% of 2-bromo-2-nitro-1, 3-propanediol; 1% of 2, 2-dibromo-3-nitrilopropionamide; and supplementing the balance of water.
And (3) sequentially putting the components into a reaction kettle, and uniformly stirring and mixing to obtain a bactericide product 4.
Comparative example 2
A bactericide comprises the following components in percentage by weight: PEG 20050%; 10% of 2-bromo-2-nitro-1, 3-propanediol; 1% of 2, 2-dibromo-3-nitrilopropionamide; and supplementing the balance of water.
And (3) sequentially putting the components into a reaction kettle, and uniformly stirring and mixing to obtain a bactericide product 5.
Performance testing
The bactericidal effect test is carried out on the bactericide products obtained in different examples and comparative examples. Adding 1-5 bactericide products into distilled water respectively, wherein the adding amount of the bactericide products is 50mg/L, stirring and uniformly mixing, and standing for 0h, 12h and 24 h. And adding equivalent bacteria liquid into the water system after standing, recording the sterilization rate for 1h, and recording the data in table 1.
TABLE 1
Examples | 0h | 12h | 24h |
Example 1 | 99.4% | 97.3% | 94.8% |
Example 2 | 99.5% | 98.1% | 96.0% |
Example 3 | 99.1% | 96.9% | 93.5% |
Comparative example 1 | 99.1% | 91.3% | 86.4% |
Comparative example 2 | 99.0% | 88.8% | 82.1% |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. A biocide, characterized in that the components comprise at least: alcohol polymer, aliphatic nitro compound, amido bond compound and halogenated compound.
2. The fungicide according to claim 1, wherein the fungicide comprises, in percentages by weight: 1-50% of alcohol polymer; 1-20% of aliphatic nitro compound; amide bond compound 0.1-5%; 0.1-5% of halogenated compound; and supplementing the balance of water.
3. The fungicide according to claim 1, wherein the fungicide comprises, in percentages by weight: 45-50% of alcohol polymer; 15-20% of aliphatic nitro compound; 0.1-1% of amido bond compound; 0.1-1% of halogenated compound; and supplementing the balance of water.
4. The bactericide according to claim 1, wherein the alcohol polymer is at least one of a polymer of monohydric alcohol, a polymer of dihydric alcohol, a polymer of trihydric alcohol, and a polymer of polyhydric alcohol.
5. The bactericidal agent of claim 4, wherein the glycol polymer is at least one selected from the group consisting of PEG200, PEG400, and PEG 600.
6. The fungicide according to claim 1, wherein said aliphatic nitro compound is at least one selected from the group consisting of 2-bromo-2-nitro-1, 3-propanediol and 2, 2-dibromo-2-nitroethanol.
7. The fungicide according to claim 1, wherein said amide bond compound is at least one selected from the group consisting of 2, 2-dibromo-3-nitrilopropionamide and 2, 2-dibromomalonamide.
8. The disinfectant according to claim 1, wherein said halogenated compound is at least one selected from the group consisting of ammonium bromide, bromoacetonitrile, potassium iodide, sodium hypochlorite, and dichlorohydantoin.
9. A method for producing a bactericide as claimed in claim 1, characterized by comprising the steps of: the components are sequentially put into a reaction kettle, and the product is obtained after uniform stirring and mixing.
10. The field of application of the fungicide according to claim 1, characterized by comprising at least: wastewater treatment, water purification, reclaimed water recycling, seawater desalination, agricultural products, leather products, furniture products, animal husbandry and aquaculture.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110152290.1A CN112868650A (en) | 2021-02-03 | 2021-02-03 | Bactericide and preparation method and application thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110152290.1A CN112868650A (en) | 2021-02-03 | 2021-02-03 | Bactericide and preparation method and application thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112868650A true CN112868650A (en) | 2021-06-01 |
Family
ID=76057165
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110152290.1A Pending CN112868650A (en) | 2021-02-03 | 2021-02-03 | Bactericide and preparation method and application thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112868650A (en) |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4732913A (en) * | 1987-02-25 | 1988-03-22 | Betz Laboratories, Inc. | Biocidal compositions and use thereof containing a synergistic mixture of 2-bromo-2-nitropropane-1,3-diol and 2,2-dibromo-3-nitrilopropionamide |
US5591759A (en) * | 1989-05-17 | 1997-01-07 | Katayama Chemical, Inc. | Aqueous isothiazolone formulation |
CN1843589A (en) * | 2006-03-20 | 2006-10-11 | 天津化工研究设计院 | Bactericide for reverse osmosis membrane and method for preparing the same |
CN102159074A (en) * | 2008-07-15 | 2011-08-17 | 陶氏环球技术公司 | Biocidal composition and method |
US20120165376A1 (en) * | 2010-12-27 | 2012-06-28 | Thomas Koehler | Stabilized microbicidal composition |
CN102548404A (en) * | 2009-09-28 | 2012-07-04 | 陶氏环球技术有限责任公司 | Compositions of dibromomalonamide and their use as biocides |
US20130184341A1 (en) * | 2009-09-28 | 2013-07-18 | Dow Global Technologies Inc. | Compositions of dibromomalonamide and their use as biocides |
CN103768956A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Reverse osmosis membrane bactericide and preparation method thereof |
CN104068028A (en) * | 2014-06-25 | 2014-10-01 | 国家海洋局天津海水淡化与综合利用研究所 | Composite bacteria and algae inhibitor and application thereof |
US20150307380A1 (en) * | 2006-02-24 | 2015-10-29 | Bromine Compounds Ltd. | Formulations containing a non-oxidative biocide and a source of active halogen and use thereof in water treatment |
CN109258668A (en) * | 2018-10-31 | 2019-01-25 | 福州盛世凌云环保科技有限公司 | A kind of high efficiency composition carbendazim Biocidal algae-killing agent and preparation method thereof |
CN112120028A (en) * | 2020-09-24 | 2020-12-25 | 新疆水处理工程技术研究中心有限公司 | Bactericide for reverse osmosis system and preparation method thereof |
-
2021
- 2021-02-03 CN CN202110152290.1A patent/CN112868650A/en active Pending
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4732913A (en) * | 1987-02-25 | 1988-03-22 | Betz Laboratories, Inc. | Biocidal compositions and use thereof containing a synergistic mixture of 2-bromo-2-nitropropane-1,3-diol and 2,2-dibromo-3-nitrilopropionamide |
US5591759A (en) * | 1989-05-17 | 1997-01-07 | Katayama Chemical, Inc. | Aqueous isothiazolone formulation |
US20150307380A1 (en) * | 2006-02-24 | 2015-10-29 | Bromine Compounds Ltd. | Formulations containing a non-oxidative biocide and a source of active halogen and use thereof in water treatment |
CN1843589A (en) * | 2006-03-20 | 2006-10-11 | 天津化工研究设计院 | Bactericide for reverse osmosis membrane and method for preparing the same |
CN102159074A (en) * | 2008-07-15 | 2011-08-17 | 陶氏环球技术公司 | Biocidal composition and method |
US20130184341A1 (en) * | 2009-09-28 | 2013-07-18 | Dow Global Technologies Inc. | Compositions of dibromomalonamide and their use as biocides |
CN102548404A (en) * | 2009-09-28 | 2012-07-04 | 陶氏环球技术有限责任公司 | Compositions of dibromomalonamide and their use as biocides |
CN102599157A (en) * | 2010-12-27 | 2012-07-25 | 罗门哈斯公司 | Stabilized microbicidal composition |
US20120165376A1 (en) * | 2010-12-27 | 2012-06-28 | Thomas Koehler | Stabilized microbicidal composition |
CN103768956A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Reverse osmosis membrane bactericide and preparation method thereof |
CN104068028A (en) * | 2014-06-25 | 2014-10-01 | 国家海洋局天津海水淡化与综合利用研究所 | Composite bacteria and algae inhibitor and application thereof |
CN109258668A (en) * | 2018-10-31 | 2019-01-25 | 福州盛世凌云环保科技有限公司 | A kind of high efficiency composition carbendazim Biocidal algae-killing agent and preparation method thereof |
CN112120028A (en) * | 2020-09-24 | 2020-12-25 | 新疆水处理工程技术研究中心有限公司 | Bactericide for reverse osmosis system and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101731257A (en) | Novel polyhexamethylene guanidine compound disinfectant and preparation method | |
CN101933521A (en) | Preparation and application thereof of sterilization composition | |
ES2765800T3 (en) | Aqueous microbicidal solutions including a monochloramine and a peracid, and methods of using the same | |
CN104068028A (en) | Composite bacteria and algae inhibitor and application thereof | |
FI66722B (en) | MEDEL MED GERMICID VERKAN FOER VATTENSYSTEM | |
CN102090413A (en) | Preparation and application of compound disinfectant | |
BRPI0808582A2 (en) | "Composition for controlling the growth of microorganisms and algae in aqueous systems and method for controlling microorganisms and algae in a water source" | |
WO2011135577A1 (en) | Polyhexamethyleneguanidine and its salts based disinfectant. | |
CN112655716A (en) | Ternary composite component efficient antibacterial antiviral treatment agent, preparation method and application thereof | |
CN105836860B (en) | A kind of stable type dioxygen aqueous disinfectant and its application in drinking water disinfection | |
CN113383775A (en) | Compound quaternary ammonium salt low-temperature disinfectant and preparation method thereof | |
CN113349201A (en) | Ethanol-gel-free no-wash disinfectant and preparation method thereof | |
JPH03501581A (en) | How to control biological contamination in recirculating water supply systems | |
MXPA02000085A (en) | Disinfectants. | |
CN108850024A (en) | A kind of composite highly effective type fungicide and preparation method thereof | |
CN113133462A (en) | Chlorine-containing disinfectant in low-temperature environment and preparation method thereof | |
CN112868650A (en) | Bactericide and preparation method and application thereof | |
CN103125510A (en) | Compound phthalic dicarboxaldehyde polyquaternium cationic surface active agent disinfectant and preparation and application thereof | |
CN108013072B (en) | High-efficiency sterilizing disinfectant and preparation method thereof | |
CN102318634A (en) | Preparation method of compound leather bactericidal and mildew-proof agent | |
CN111919854A (en) | Rare earth disinfectant for sterilizing and relieving itching | |
CN102318635A (en) | Preparation method of compound leather bactericidal and mildew-proof agent | |
JP2003519161A (en) | Stabilized isothiazolone composition and method for stabilizing isothiazolone | |
CN104082293B (en) | A kind of composite alcohol sterilizing agent and its preparation method | |
CN111374150A (en) | Preparation method of nano-silver/hydrogen peroxide/salicylic acid composite disinfection material |
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 |