CN110950726A - Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof - Google Patents

Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof Download PDF

Info

Publication number
CN110950726A
CN110950726A CN201911321950.3A CN201911321950A CN110950726A CN 110950726 A CN110950726 A CN 110950726A CN 201911321950 A CN201911321950 A CN 201911321950A CN 110950726 A CN110950726 A CN 110950726A
Authority
CN
China
Prior art keywords
powder
dicyandiamide
polyurethane adhesive
sulfur
smokeless
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
Application number
CN201911321950.3A
Other languages
Chinese (zh)
Inventor
刘吉平
阮方
于保藏
李琪军
刘克普
吉伟生
周耀明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Jirun Fireworks New Material Technology Co Ltd
Original Assignee
Jiangxi Jirun Fireworks New Material Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jiangxi Jirun Fireworks New Material Technology Co Ltd filed Critical Jiangxi Jirun Fireworks New Material Technology Co Ltd
Priority to CN201911321950.3A priority Critical patent/CN110950726A/en
Publication of CN110950726A publication Critical patent/CN110950726A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B27/00Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C06EXPLOSIVES; MATCHES
    • C06BEXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B23/00Compositions characterised by non-explosive or non-thermic constituents
    • C06B23/009Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up

Abstract

The invention relates to a smokeless and sulfur-free firework display bomb lift-off agent and a preparation method thereof, and belongs to the technical field of civil entertainment fireworks. Weighing nitrocellulose, dicyandiamide, sepiolite fiber powder, titanium hydride powder, rare earth photoluminescence powder and polyurethane adhesive; dividing the polyurethane adhesive into three parts; dissolving dicyandiamide in hot water to prepare dicyandiamide solution, spraying the solution on the sepiolite fiber powder while turning over, dripping a first portion of polyurethane adhesive into the solution after drying, grinding and sieving to obtain dicyandiamide/sepiolite fiber powder. Mixing titanium hydride powder and rare earth photoluminescence powder, dripping a second part of polyurethane adhesive, sieving and drying to obtain the luminescence granulation powder. Mixing nitrocellulose, dicyandiamide/sepiolite fiber powder and luminous granulation powder, dripping a third polyurethane adhesive, kneading, drying, grinding, sieving and granulating to obtain the smokeless and sulfur-free firework bomb lift-off medicament. The invention provides a smokeless and sulfur-free firework bomb lift-off agent which has good stability, low cost and green and environment-friendly setting off process.

Description

Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof
Technical Field
The invention relates to a smokeless and sulfur-free firework display bomb lift-off agent and a preparation method thereof, and belongs to the technical field of civil entertainment fireworks.
Background
The display shell is one of the most popular fireworks, plays an important role in rendering joyful atmosphere in large-scale performance, presents various patterns and a flawless effect after being launched into the air, and greatly meets the ornamental requirements of people.
However, the traditional display shell is in a severe development embarrassment nowadays, and because the main component of the traditional display shell is black powder, the stability is poor, and safety accidents occurring when the display shell is set off are rare, so that great loss is caused to the property and life safety of people. Meanwhile, the display shell generates serious dust and pungent smell in the setting-off process, pollutes the living environment and is contrary to the current trend of environmental protection.
The government has become more and more strict in the standards for the production and setting off of fireworks, issues banning orders related to the compulsory implementation of fireworks, and strictly prohibits the setting off of display shells in many areas. Therefore, the firework display bomb lift-off agent which is green, environment-friendly and excellent in stability is an urgent need in the firework industry, and has important commercial value and social significance.
Disclosure of Invention
The invention aims to solve the problems of poor safety, serious pollution and the like of the conventional aerial shell lift-off medicament, and provides a smokeless and sulfur-free aerial shell lift-off medicament and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme.
A smokeless and sulfur-free firework shell lift-off medicament comprises the following components in parts by mass:
Figure BDA0002327381110000011
Figure BDA0002327381110000021
the particle size of the nitrocellulose is less than or equal to 150 mu m.
The particle size of the dicyandiamide is less than or equal to 100 mu m.
The particle size of the sepiolite fiber powder is less than or equal to 100 mu m.
The particle size of the titanium hydride powder is less than or equal to 50 mu m.
The rare earth luminescent powder can emit red, bright yellow or blue light with different colors, and the particle size is less than or equal to 80 mu m.
A smokeless and sulfur-free firework bomb lift-off medicament and a preparation method thereof comprise the following specific steps:
weighing nitrocellulose, dicyandiamide, sepiolite fiber powder, titanium hydride powder, rare earth photoluminescence powder and polyurethane adhesive according to a formula proportion.
And step two, dividing the polyurethane adhesive into three parts, wherein the first part is 0.1-0.5% of the total mass of dicyandiamide and sepiolite fiber powder, the second part is 0.1-0.5% of the total mass of titanium hydride powder and rare earth photoluminescence powder, and the rest is the third part.
Dissolving dicyandiamide in hot water at 60 ℃ to prepare dicyandiamide solution, filling the solution into a spray can, and spraying the solution onto evenly spread sepiolite fiber powder; stirring the sepiolite fiber powder while spraying to ensure uniform spraying; and after spraying, placing the mixture in an oven at 120 ℃ for vacuum drying for 4 hours, dropwise adding a first polyurethane adhesive into the mixture, kneading uniformly, drying, grinding and sieving to obtain dicyandiamide/sepiolite fiber powder.
And step four, uniformly mixing the titanium hydride powder and the rare earth photoluminescence powder, dripping a second part of polyurethane adhesive, kneading, uniformly sieving and drying to obtain the luminescent granulation powder.
And step five, uniformly mixing the nitrocellulose weighed in the step one, the dicyandiamide/sepiolite fiber powder prepared in the step three and the light-emitting granulation powder prepared in the step four, dropwise adding a third polyurethane adhesive, uniformly kneading, drying, grinding, sieving and granulating to obtain the smokeless and sulfur-free firework shell lift-off medicament.
Advantageous effects
1. The smokeless and sulfur-free aerial shell lift-off agent provided by the invention has good stability and excellent safety performance in the processes of production, storage and transportation. The raw materials required by the preparation are low in cost and easy to obtain; the setting off process is smokeless and sulfur-free, and green and environment-friendly.
2. The smokeless and sulfur-free firework display bomb lift-off agent provided by the invention selects different rare earth photoluminescence powder, and the firework display bomb can present colorful fireworks and has great ornamental value.
3. The smokeless and sulfur-free aerial shell lift-off medicament and the preparation method thereof provided by the invention have the advantages of mature and stable preparation process, no pollution in the production process and suitability for large-scale industrial production.
Detailed Description
The following examples are given in conjunction with the experimental results of the present invention to further illustrate the invention as example 1:
a smokeless and sulfur-free firework shell lift-off medicament comprises the following components in parts by mass:
Figure BDA0002327381110000031
a smokeless and sulfur-free firework bomb lift-off medicament comprises the following specific steps:
weighing 150g of nitrocellulose, 25g of dicyandiamide, 10g of sepiolite fiber powder, 50g of titanium hydride powder, 12.5g of red rare earth photoluminescence powder and 2.5g of polyurethane adhesive according to the formula proportion.
The polyurethane adhesive was divided into three portions, a first portion of 0.16g, a second portion of 0.24g and a third portion of 2.1 g.
Dissolving dicyandiamide in hot water at 60 ℃ to prepare dicyandiamide solution, filling the solution into a spray can, and spraying the solution on evenly spread sepiolite fiber powder; stirring the sepiolite fiber powder while spraying to ensure uniform spraying; after spraying, the mixture is placed in an oven at 120 ℃ for vacuum drying for 4 hours, a first portion of polyurethane adhesive is dropwise added into the mixture at the rate of 5 drops/min, the mixture is kneaded for 10 minutes until the system is uniform, the mixture is dried at 30 ℃ for 4 hours in vacuum, and the mixture is ground and sieved by a 100-mesh sieve to obtain 34.97g of dicyandiamide/sepiolite fiber powder.
Uniformly mixing titanium hydride powder and red rare earth photoluminescence powder, dripping a second part of polyurethane adhesive at the speed of 5 drops/min, kneading for 15min until the system is uniform, sieving by a 100-mesh sieve, and drying at 30 ℃ for 5h to obtain 62.62g of luminous granulation powder.
Uniformly mixing nitrocellulose, dicyandiamide/sepiolite fiber powder and luminescent granulation powder, starting to dropwise add a third polyurethane adhesive at the speed of 10 drops/min, kneading for granulation for 30min after dropwise addition, carrying out vacuum drying for 6h at 40 ℃, sieving with a 100-mesh sieve after grinding, and carrying out granulation to obtain 239.73g of smokeless and sulfur-free firework bomb lift-off medicament.
The prepared smokeless and sulfur-free aerial shell lift-off medicament has good stability, 10 plus or minus 0.1g of smokeless and sulfur-free aerial shell lift-off medicament is accurately weighed in a beaker and placed in a safe constant-temperature oven at the temperature of 75 plus or minus 2 ℃ for 48 hours, and a sample is non-combustible and non-explosive; the lowest explosion height of the display shell prepared by the agent is higher than 60m, and the highest explosion height is lower than 100 m; and the setting off process has no smoke, sulfur and scorching residues, and the flame is red.
Example 2:
a smokeless and sulfur-free firework shell lift-off medicament comprises the following components in parts by mass:
Figure BDA0002327381110000041
a smokeless and sulfur-free firework bomb lift-off medicament comprises the following specific steps:
370g of nitrocellulose, 111g of dicyandiamide, 59.2g of sepiolite fiber powder, 185g of titanium hydride powder, 74g of bright yellow rare earth photoluminescence powder and 14.8g of polyurethane adhesive are weighed according to the formula proportion.
The polyurethane adhesive was divided into three portions, a first portion of 0.6g, a second portion of 1.2g and a third portion of 13 g.
Dissolving dicyandiamide in hot water at 60 ℃ to prepare dicyandiamide solution, filling the solution into a spray can, and spraying the solution on evenly spread sepiolite fiber powder; stirring the sepiolite fiber powder while spraying to ensure uniform spraying; after spraying, the mixture is placed in an oven at 120 ℃ for vacuum drying for 4 hours, a first portion of polyurethane adhesive is dropwise added into the mixture at the speed of 10 drops/min, the mixture is kneaded for 15 minutes until the system is uniform, the mixture is dried at 35 ℃ for 2 hours in vacuum, and the mixture is ground and sieved by a 120-mesh sieve to obtain 170.46g of dicyandiamide/sepiolite fiber powder.
Uniformly mixing titanium hydride powder and bright yellow rare earth photoluminescence powder, dripping a second part of polyurethane adhesive at the speed of 10 drops/min, kneading for 20min until the system is uniform, sieving by a 120-mesh sieve, and drying at 35 ℃ for 3h to obtain 260.14g of luminous granulation powder.
Uniformly mixing nitrocellulose, dicyandiamide/sepiolite fiber powder and luminescent granulation powder, starting to dropwise add a third polyurethane adhesive at the rate of 15 drops/min, kneading for 40min for granulation, carrying out vacuum drying at 45 ℃ for 3h, grinding, sieving with a 120-mesh sieve, and carrying out granulation to obtain 732.35g of smokeless and sulfur-free firework bomb lift-off medicament.
The prepared smokeless and sulfur-free aerial shell lift-off medicament has good stability, 10 plus or minus 0.1g of smokeless and sulfur-free aerial shell lift-off medicament is accurately weighed in a beaker and placed in a safe constant-temperature oven at the temperature of 75 plus or minus 2 ℃ for 48 hours, and a sample is non-combustible and non-explosive; the lowest explosion height of the display shell prepared by the agent is higher than 60m, and the highest explosion height is lower than 100 m; and the flame is bright yellow without smoke, sulfur and burning residues in the setting-off process.
Example 3:
a smokeless and sulfur-free firework shell lift-off medicament comprises the following components in parts by mass:
Figure BDA0002327381110000051
Figure BDA0002327381110000061
a smokeless and sulfur-free firework bomb lift-off medicament comprises the following specific steps:
weighing 1.6kg of nitrocellulose, 1.2kg of dicyandiamide, 0.2kg of sepiolite fiber powder, 0.6kg of titanium hydride powder, 0.28kg of blue rare earth photoluminescence powder and 0.12kg of polyurethane adhesive according to the formula proportion.
The polyurethane adhesive was divided into three portions, a first portion of 5.7g, a second portion of 4.3g and a third portion of 110 g.
Dissolving dicyandiamide in hot water at 60 ℃ to prepare dicyandiamide solution, filling the solution into a spray can, and spraying the solution on evenly spread sepiolite fiber powder; stirring the sepiolite fiber powder while spraying to ensure uniform spraying; after spraying, the mixture is placed in an oven at 120 ℃ for vacuum drying for 4 hours, a first portion of polyurethane adhesive is dropwise added into the mixture at the speed of 10 drops/min, the mixture is kneaded for 20 minutes until the system is uniform, the mixture is dried in vacuum at 40 ℃ for 2 hours, and the mixture is ground and sieved by a 150-mesh sieve to obtain 1403.7g of dicyandiamide/sepiolite fiber powder.
Uniformly mixing titanium hydride powder and bright yellow rare earth photoluminescence powder, dripping a second part of polyurethane adhesive at the speed of 15 drops/min, kneading for 30min until the system is uniform, sieving by a 150-mesh sieve, and drying at 40 ℃ for 2h to obtain 883.65g of luminous granulation powder.
Uniformly mixing nitrocellulose, dicyandiamide/sepiolite fiber powder and luminescent granulation powder, starting to dropwise add a third part of polyurethane adhesive at the rate of 20 drops/min, kneading for granulation for 45min after dropwise addition, carrying out vacuum drying for 2h at 50 ℃, sieving with a 150-mesh sieve after grinding, and carrying out granulation to obtain 3.98kg of smokeless and sulfur-free firework bomb lift-off medicament.
The prepared smokeless and sulfur-free aerial shell lift-off medicament has good stability, 10 plus or minus 0.1g of smokeless and sulfur-free aerial shell lift-off medicament is accurately weighed in a beaker and placed in a safe constant-temperature oven at the temperature of 75 plus or minus 2 ℃ for 48 hours, and a sample is non-combustible and non-explosive; the lowest explosion height of the display shell prepared by the agent is higher than 60m, and the highest explosion height is lower than 100 m; and the setting off process has no smoke, sulfur and scorching residues, and the flame is blue.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. The smokeless and sulfur-free firework display bomb lift-off agent is characterized in that: the formula comprises the following components in percentage by mass:
Figure FDA0002327381100000011
2. the medicament of claim 1, wherein: the particle size of the nitrocellulose is less than or equal to 150 mu m.
3. The medicament of claim 1, wherein: the particle size of the dicyandiamide is less than or equal to 100 mu m.
4. The medicament of claim 1, wherein: the particle size of the sepiolite fiber powder is less than or equal to 100 mu m.
5. The medicament of claim 1, wherein: the particle size of the titanium hydride powder is less than or equal to 50 mu m.
6. The medicament of claim 1, wherein: the grain diameter of the color rare earth luminescent powder is less than or equal to 80 mu m.
7. The medicament of claim 6, wherein: the color rare earth luminescent powder can emit light with different colors such as red, bright yellow or blue.
8. The method of launching a smokeless and sulfur-free display shell of claim 1, wherein: the method comprises the following specific steps:
weighing nitrocellulose, dicyandiamide, sepiolite fiber powder, titanium hydride powder, rare earth photoluminescence powder and polyurethane adhesive according to a formula ratio;
dividing the polyurethane adhesive into three parts, wherein the first part is 0.1-0.5% of the total mass of dicyandiamide and sepiolite fiber powder, the second part is 0.1-0.5% of the total mass of titanium hydride powder and rare earth photoluminescence powder, and the rest is the third part;
dissolving dicyandiamide in hot water at 60 ℃ to prepare dicyandiamide solution, filling the solution into a spray can, and spraying the solution onto evenly spread sepiolite fiber powder; stirring the sepiolite fiber powder while spraying to ensure uniform spraying; after spraying, placing the mixture in a drying oven at 120 ℃ for vacuum drying for 4 hours, dripping a first polyurethane adhesive into the mixture, kneading the mixture uniformly, drying the mixture, grinding the mixture and sieving the ground mixture to obtain dicyandiamide/sepiolite fiber powder;
step four, uniformly mixing titanium hydride powder and rare earth photoluminescence powder, dripping a second part of polyurethane adhesive, kneading, uniformly sieving and drying to obtain luminous granulation powder;
and step five, uniformly mixing the nitrocellulose weighed in the step one, the dicyandiamide/sepiolite fiber powder prepared in the step three and the light-emitting granulation powder prepared in the step four, dropwise adding a third polyurethane adhesive, uniformly kneading, drying, grinding, sieving and granulating to obtain the smokeless and sulfur-free firework shell lift-off medicament.
CN201911321950.3A 2019-12-20 2019-12-20 Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof Pending CN110950726A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911321950.3A CN110950726A (en) 2019-12-20 2019-12-20 Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911321950.3A CN110950726A (en) 2019-12-20 2019-12-20 Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110950726A true CN110950726A (en) 2020-04-03

Family

ID=69982907

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911321950.3A Pending CN110950726A (en) 2019-12-20 2019-12-20 Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110950726A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111912300A (en) * 2020-08-04 2020-11-10 北京理工大学 Stability treatment method of nitrated bamboo cellulose paper

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215211A (en) * 2007-01-04 2008-07-09 邹建文 Smokeless flameless gunpowder agent
GB2472648A (en) * 2009-08-14 2011-02-16 John Douglas Michael Wraige Pyrotechnic composition and device
CN103121886A (en) * 2012-12-26 2013-05-29 南京理工大学 Multicolor cold-firework reagent and manufacturing method of cold fireworks
CN104276908A (en) * 2013-07-10 2015-01-14 周健 Safe environment-friendly novel pyrotechnic composition
CN104944423A (en) * 2015-06-10 2015-09-30 北京理工大学 High-energy-point gunpowder and preparation method
CN108299135A (en) * 2018-01-29 2018-07-20 泸州北方化学工业有限公司 A kind of smokelessly cold light firework medicament without ammonia odor
CN108997073A (en) * 2018-08-30 2018-12-14 浏阳市万盛烟花制造有限公司 It is a kind of to prepare the modified bentonite composite of safe firework medicament in improvement

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215211A (en) * 2007-01-04 2008-07-09 邹建文 Smokeless flameless gunpowder agent
GB2472648A (en) * 2009-08-14 2011-02-16 John Douglas Michael Wraige Pyrotechnic composition and device
CN103121886A (en) * 2012-12-26 2013-05-29 南京理工大学 Multicolor cold-firework reagent and manufacturing method of cold fireworks
CN104276908A (en) * 2013-07-10 2015-01-14 周健 Safe environment-friendly novel pyrotechnic composition
CN104944423A (en) * 2015-06-10 2015-09-30 北京理工大学 High-energy-point gunpowder and preparation method
CN108299135A (en) * 2018-01-29 2018-07-20 泸州北方化学工业有限公司 A kind of smokelessly cold light firework medicament without ammonia odor
CN108997073A (en) * 2018-08-30 2018-12-14 浏阳市万盛烟花制造有限公司 It is a kind of to prepare the modified bentonite composite of safe firework medicament in improvement

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
中国医药集团上海化学试剂公司: "《试剂手册》", 30 November 2002, 上海科学技术出版社 *
张占立: "《常用金属材料手册》", 31 October 2012, 河南科学技术出版社 *
王淑芬: "《化学故事》", 30 April 2013, 吉林教育出版社 *
范存善等: "海泡石的性质及用途", 《化工之友》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111912300A (en) * 2020-08-04 2020-11-10 北京理工大学 Stability treatment method of nitrated bamboo cellulose paper
CN111912300B (en) * 2020-08-04 2021-07-20 北京理工大学 Stability treatment method of nitrated bamboo cellulose paper

Similar Documents

Publication Publication Date Title
CN103121886B (en) Multicolor cold-firework reagent and manufacturing method of cold fireworks
CN103030483B (en) Bright green cold firework composition and production method thereof
CN104829401B (en) A kind of safety and environmental protection colorful firecrackers medicament and the method for preparing colorful firecrackers with the medicament
CN104276908A (en) Safe environment-friendly novel pyrotechnic composition
CN103435429B (en) Environment-friendlyfirework firework propellant
CN104973998A (en) Firework gunpowder composition for firework sounding beads
CN110981666A (en) Smokeless and sulfur-free golden indoor setting-off type cold firework explosive and preparation method thereof
CN110950726A (en) Smokeless and sulfur-free firework bomb lift-off agent and preparation method thereof
CN111620756A (en) Formula and preparation process of bright bead for fireworks
CN110981669A (en) Low-sensitivity environment-friendly firework chemical and preparation method thereof
CN110343027B (en) Chlorine-free orange pyrotechnic agent based on energetic metal organic framework and preparation method thereof
CN107793280B (en) Composite type insensitive agent for firework powder
CN104529682A (en) Environment-friendly propellant
CN111018640A (en) Stabilizing treatment and preparation method of high-explosive-sound smokeless sulfur-free firecracker nitrate medicament
CN111440039A (en) Novel indoor and outdoor cold firework formula and preparation process thereof
CN105330498A (en) Colorful firework and preparation method thereof
CN100405000C (en) Smokeless fireworks
CN100445241C (en) Flash corolla star for fireworks and its making method
CN109721446B (en) Micro-pyrotechnic composition and application thereof
RU2549865C1 (en) Pyrotechnic composition of colour of fire
CN105330497A (en) Colorful firework and preparation method thereof
CN201463726U (en) Firework shell for setting off special-effect fireworks
CN111039731A (en) Color light cold firework chemical and preparation method thereof
CN110963864A (en) Low-sensitivity smokeless and sulfur-free firecracker nitrate medicament and preparation method thereof
CN1420109A (en) Blue light agent

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200403