CN107674459A - The method that pigment hydrolyzes coating - Google Patents
The method that pigment hydrolyzes coating Download PDFInfo
- Publication number
- CN107674459A CN107674459A CN201710890667.7A CN201710890667A CN107674459A CN 107674459 A CN107674459 A CN 107674459A CN 201710890667 A CN201710890667 A CN 201710890667A CN 107674459 A CN107674459 A CN 107674459A
- Authority
- CN
- China
- Prior art keywords
- pigment
- electrolyser
- source
- cathode chamber
- anode
- 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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/405—Compounds of aluminium containing combined silica, e.g. mica
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
Abstract
The present invention relates to a kind of method of pigment hydrolysis coating, the reactor of use includes electrolyser and dc source；Cathode chamber and anode chamber are divided into by anion-exchange membrane in the electrolyser, the inert cathode being connected with the negative pole of dc source is provided with the cathode chamber；The anode being connected with the positive pole of dc source is provided with the anode chamber；Agitating paddle is provided with the cathode chamber and is communicated with the disturbed flow pipe of woven hose thereon, and the flow-disturbing tube wall is provided with multiple holes；Add water that suspension is made pigment base material, and be put into the cathode chamber of electrolyser, start agitating paddle；Then required deposition agent is passed sequentially through into woven hose to add in cathode chamber, and by controlling the size of current of dc source to control the pH value in electrolyser in the range of needs, until hydrolysis terminates so that deposition agent deposits the surface for being coated on pigment base material.It is undesirable that the present invention solves the hydrolysis coating process reaction condition control of existing pigment, the problem of need to additionally adding buffer solution.
Description
Technical field
The invention belongs to pigment production technical field, and in particular to a kind of pigment applied to fields such as cosmetics, ink
Hydrolysis coating method.
Background technology
Production technology applied to the pigment in the fields such as cosmetics, ink generally comprises the calcining, removal of impurities, drift of base material
Wash, mill, disperseing, rough segmentation, acid treatment, alkali process, essence point, hydrolysis coating, washing filter, drying calcining etc. technique, it is therein
Some techniques can be deleted or increased according to different needs, but hydrolysis coating therein（Coated in substrate surface
One layer of index of refraction and the larger film of base material difference）This technique is essential, and its quality to pigment plays key
The effect of property.And the hydrolysis coating process of pigment is to the reaction condition of hydrolyzation system（Such as pH value, temperature, mixing effect）Control will
Ask very high, the hydrolysis coating effect that the fluctuation of reaction condition can be to pigment makes a big impact, so as to influence the quality of pigment.
At present, the hydrolysis coating process of pigment is covered to complete typically by some strong acid weak base salt hydrolytic precipitations are added
, but generally along with the decline of H+ generation, i.e. pH value during such strong acid weak base salt hydrolytic precipitation, such as it is the most frequently used
TiCl4, it is as follows that it hydrolyzes equation：
TiCl4 + (x+2)H2O = TiO2•xH2O↓ + 4HCl；
HCl caused by hydrolysis can substantially reduce system pH, and pH value, which reduces, can suppress titanium tetrachloride and continue to hydrolyze, and cause coating
Inequality, influence the quality of pigment.For this reason, it may be necessary in the hydrolytic process add NaOH in and HCl.But due to acid-base neutralization reaction
It is rapid and acutely, existing based on adding the flow control of reactor pair plus alkali that alkali neutralisation is principle to require high, flow
The slight errors of control are that can cause the big ups and downs of pH value, while alkali lye has higher corrosivity.Therefore to such reaction
The accurate control of alkali lye conveying control reactor requires very high with corrosion-resistant in device, and reactor price is high.Simultaneously because soda acid
The severity of neutralization reaction and heat release, adding alkali neutralisation easily to cause the mouth of pipe, nearby pH value and temperature are above away from spout part
The region of position, reaction condition is uneven everywhere for system.In the case of many pH stability and uniformity requirement are higher, add alkali neutralizing hydrolysis
The reaction condition of coating reactor controls unsatisfactory, it is necessary to additionally add buffer solution regulation and control pH value, on the one hand improves materials
Cost, another aspect buffer solution cause pollution to reaction solution, improve environmentally friendly cost.
The content of the invention
The invention provides a kind of method of pigment hydrolysis coating, and it can solve existing pigment hydrolysis coating process and deposit
Undesirable, the problem of need to additionally adding buffer solution is controlled in reaction condition.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
Coating is hydrolyzed using pigment hydrolysis coating reactor in it, and the reactor includes electrolyser and dc source；It is described
Cathode chamber and anode chamber are divided into by anion-exchange membrane in electrolyser, the negative pole phase with dc source is provided with the cathode chamber
Inert cathode even；The anode being connected with the positive pole of dc source is provided with the anode chamber；Stirring is provided with the cathode chamber
Oar and the disturbed flow pipe for being communicated with woven hose thereon, the flow-disturbing tube wall are provided with multiple holes；
This method includes step in detail below：
Add water that suspension is made pigment base material, and be put into the cathode chamber of electrolyser, start agitating paddle；Then by required deposition
Agent passes sequentially through woven hose and added in cathode chamber, and by controlling the size of current of dc source to control the pH value in electrolyser to exist
In the range of needing, until hydrolysis terminates so that deposition agent deposits the surface for being coated on pigment base material.
In above-mentioned technical proposal, more specifically technical scheme can also be：The inert cathode is spirally coiled in disturbed flow pipe
On.
Further, the anode is iron or ferroalloy materials.
Due to using above-mentioned technical proposal, the beneficial effect that the present invention obtains is：
1 present invention has abandoned traditional alkali neutralisation that adds, and whole process reacts the alkali lye without using highly corrosive, by being sent out in electrolyser
Reactor, i.e., be powered, utilized by H+ caused by raw electrochemical method consumption hydrolysis in course of reaction using constant voltage dc source
Cathode reaction 2H++2e-=H2 ↑, H+ caused by hydrolyzate hydrolysis is constantly consumed, is replaced by the size of current for adjusting dc source
The flux of alkaline liquor of tradition plus alkali neutralisation control consumption H+ speed, makes its consumption H+ speed consistent with hydrolysis rate, therefore,
Its course of reaction is relatively mild controllable（Control electric current size is simpler more easy to operate than control uninterrupted）, to reactor requirement
It is relatively low, it is cheap；Meanwhile multiple apertures are provided with disturbed flow pipe, after deposition agent enters reaction system by the aperture of disturbed flow pipe
I.e. under the drive of agitating paddle around screw electrode rotate, while disturbed flow pipe can appropriate flow-disturbing, ensure hydrolyzate can be with electricity
Extremely uniformly sufficiently contact, the pH value of reaction system is further stabilized, therefore during the hydrolysis cladding of whole pigment simultaneously
Buffer solution need not be additionally added, has saved great amount of cost.
2. inert cathode is spirally coiled in disturbed flow pipe by the present invention, allow reaction solution uniformly to mix, and make reaction solution with stirring
The startup for mixing oar fully contacts with electrode and heating tube, and reaction system uniformly can heat and consume everywhere H+, further solution
The problem of pH and temperature distributing disproportionation be present in tradition of having determined plus alkali neutralization reaction device.
3. electrolyser negative electrode chamber outer wall of the present invention is anion-exchange membrane, chlorion caused by hydrolysis can be during the course of the reaction
Anode region is reached through anion-exchange membrane, its Anodic is iron and ferroalloy materials, iron and ferroalloy material in course of reaction
Material dissolving enters solution, and ferrous solution is generated with chlorion, and carries out recycling ferric chloride solution, and ferric chloride solution is exactly
The important source material of iron system pearlescent pigment production；In addition, the waste liquid of cathodic region reaction solution after filtering due to containing substantial amounts of chlorine from
Son, therefore can be recovered and for producing ferric chloride solution, realize the recycling of waste.
Brief description of the drawings
Fig. 1 is the structural representation of equipment used by pigment of the present invention hydrolysis coating.
Embodiment
In order to better illustrate the present invention, below in conjunction with drawings and the specific embodiments, the invention will be further described, and
Protection scope of the present invention is not intended to be limited to following examples.
As shown in Fig. 1 the pigment hydrolysis coating reactor that the present invention uses, it includes electrolyser 1 and dc source
6；Cathode chamber 3 and anode chamber 4 are divided into by anion-exchange membrane 2 in the electrolyser 1, are provided with the cathode chamber 3 and direct current
The connected inert cathode 5 of the negative pole of power supply 6；The anode 7 being connected with the positive pole of dc source 6 is provided with the anode chamber 4；It is described
The disturbed flow pipe 9 of woven hose 10 is communicated with cathode chamber 3 provided with agitating paddle 8 and its upper end；The disturbed flow pipe 9 is provided with multiple holes 11,
Deposition agent is entered after reaction system by multiple holes 11 on disturbed flow pipe 7 to be rotated under the drive of agitating paddle 8 around screw electrode,
Simultaneously disturbed flow pipe 7 can appropriate flow-disturbing, ensure hydrolyzate uniformly can sufficiently be contacted with electrode；The spiral of inert cathode 3
It is coiled on disturbed flow pipe 9, allows reaction solution uniformly to mix, and reaction solution is filled with the startup of agitating paddle 8 with electrode and heating tube
Tap is touched, and reaction system uniformly can heat and consume everywhere H+；The anode 7 is iron and ferroalloy materials, in course of reaction
Iron and ferroalloy materials dissolving enter solution, and ferrous solution, recyclable recycling are generated with chlorion；
The method of pigment hydrolysis coating of the present invention includes step in detail below：
Add water that suspension is made pigment base material, and be put into the cathode chamber 3 of electrolyser 1, start agitating paddle 8；Then by needed for
Deposition agent passes sequentially through woven hose 10 and added in cathode chamber 3, and by controlling the size of current of dc source 6 to control electrolyser 1
Interior pH value is in the range of needs, until hydrolysis terminates so that deposition agent deposits the surface for being coated on pigment base material.
Embodiment
Golden serial low-luster uses equipment as shown in Figure 1 with the hydrolysis coating method of piece layer pigment, and it includes
Electrolyser 1 and dc source 6；Wherein, cathode chamber 3 and anode chamber are separated into by anion-exchange membrane 2 among the electrolyser 1
4, there is inert cathode 5 in the cathode chamber 3, be connected with the negative pole of dc source 6；There is anode 7 in the anode chamber 4, with direct current
The positive pole of power supply 6 is connected；There are agitating paddle 8 and disturbed flow pipe 9 in the cathode chamber 3, the upper end of the disturbed flow pipe 9 is communicated with woven hose
10；The disturbed flow pipe 9 is provided with multiple holes 11, and the inert cathode 3 is spirally coiled on disturbed flow pipe 9, and the anode 7 is iron and iron
Alloy material；
Golden serial low-luster includes step in detail below with the hydrolysis coating method of piece layer pigment：
A. by base material mica powder and crystal grain conditioning agent input deionized water, suspension is made, is then placed in the negative electrode of electrolyser 1
In room 3, start agitating paddle 8；Wherein, the dosage of the crystal grain conditioning agent is the 0.01%~2% of mica powder quality；
B. the size of current of dc source 6 is adjusted, the pH value of the suspension is maintained at 1.5, is then added from woven hose 10
The SnCl of the mica powder quality 0.5%4·5H2O solution, and made in the process by adjusting the size of current of dc source 6
Its pH value keeps constant；As the SnCl4·5H2After the addition of O solution terminates, continue constant temperature and stir 15 minutes~30 minutes；
C. the size of current of dc source 6 is adjusted, the pH value of the suspension is adjusted to 1.8~2.0, then from woven hose 10
Add TiCl4Solution is changed into weak golden up to the color of the suspension, and in the process again by regulation dc source 6
Size of current make its pH value keep it is constant；As the TiCl4After solution addition terminates, continue constant temperature and stir 15 minutes~30 points
Clock；
D. the size of current of dc source 6 is adjusted, the pH value of the suspension is adjusted 2.5~3.3, then again from woven hose
10 add FeCl3Solution is changed into required form and aspect up to the color of the suspension, and in the process again by regulation direct current
The size of current of power supply 6 makes its pH value keep constant.
Comparison example
The hydrolysis coating method of golden serial low-luster piece layer pigment comprises the following steps：
A. by base material mica powder and crystal grain conditioning agent input deionized water, suspension is made；Wherein, the crystal grain conditioning agent
Dosage is the 0.01%~2% of mica powder quality；
B. the pH value of this suspension is adjusted to 1.5 with watery hydrochloric acid, then add the SnCl of the mica powder quality 0.5%4·
5H2O solution, and 20% sodium hydroxide is added dropwise in the process to keep pH value constant；As the SnCl4·5H2O solution addition knot
Shu Hou, continue constant temperature and stir 15 minutes~30 minutes；
C. the pH value of this suspension is adjusted to 1.8~2.0 with watery hydrochloric acid, then adds TiCl4Solution is until the suspension
Color be changed into weak golden, and 20% sodium hydroxide is added dropwise in the process to keep pH value constant；As the TiCl4Solution adds
After adding end, continue constant temperature and stir 15 minutes~30 minutes；
D. the pH value of this suspension is adjusted to 2.5~3.3 with watery hydrochloric acid, then adds FeCl3Solution is until the suspension
Color be changed into required form and aspect, and 20% sodium hydroxide is added dropwise in the process to keep pH value constant.
The result of above-described embodiment and comparison example is compared, finds relative and comparison example, the present invention is implemented
Example reaction system is more prone to control, and without additionally adding buffer solution again.
Claims (3)
- A kind of 1. method of pigment hydrolysis coating, it is characterised in that：Coating is hydrolyzed using pigment hydrolysis coating reactor, should Reactor includes electrolyser（1）And dc source（6）；The electrolyser（1）Inside pass through anion-exchange membrane（2）It is divided into negative electrode Room（3）And anode chamber（4）, the cathode chamber（3）Inside it is provided with and dc source（6）The connected inert cathode of negative pole（5）；It is described Anode chamber（4）Inside it is provided with and dc source（6）The connected anode of positive pole（7）；The cathode chamber（3）It is interior to be provided with agitating paddle（8） Woven hose is communicated with thereon（10）Disturbed flow pipe（9）, the disturbed flow pipe（9）Wall is provided with multiple holes（11）；This method includes step in detail below：Add water that suspension is made pigment base material, and be put into electrolyser（1）Cathode chamber（3）It is interior, start agitating paddle（8）；Then Required deposition agent is passed sequentially through into woven hose（10）Add cathode chamber（3）It is interior, and by controlling dc source（6）Size of current Control electrolyser（1）Interior pH value is in the range of needs, until hydrolysis terminates so that deposition agent deposition is coated on pigment The surface of base material.
- 2. the method for pigment hydrolysis coating according to claim 1, it is characterised in that：The inert cathode（5）Helical disk It is wound on disturbed flow pipe（9）On.
- 3. the method for pigment hydrolysis coating according to claim 1 or 2, it is characterised in that：The anode is that iron or iron close Golden material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710890667.7A CN107674459A (en) | 2017-09-27 | 2017-09-27 | The method that pigment hydrolyzes coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710890667.7A CN107674459A (en) | 2017-09-27 | 2017-09-27 | The method that pigment hydrolyzes coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107674459A true CN107674459A (en) | 2018-02-09 |
Family
ID=61137574
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710890667.7A Pending CN107674459A (en) | 2017-09-27 | 2017-09-27 | The method that pigment hydrolyzes coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107674459A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462197A (en) * | 2021-06-30 | 2021-10-01 | 常熟世名化工科技有限公司 | Preparation method of titanium dioxide aqueous dispersion, product and application thereof |
| CN115260796A (en) * | 2022-08-11 | 2022-11-01 | 福建坤彩材料科技股份有限公司 | Pearlescent pigment and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN104120459A (en) * | 2014-08-06 | 2014-10-29 | 哈尔滨工业大学 | Preparation method of iron-based oxide colored pigment |
| CN104477950A (en) * | 2014-12-09 | 2015-04-01 | 四川大学 | Method for preparing high-purity alkaline magnesium carbonate and calcium carbonate by means of CO2 mineralization of dolomite |
| CN105542517A (en) * | 2016-01-14 | 2016-05-04 | 广西七色珠光材料股份有限公司 | White and interference-color matte flaky cored pigment and preparation method thereof |
| CN107019141A (en) * | 2017-06-01 | 2017-08-08 | 稻思（上海）纳米科技有限公司 | One kind is thrown into the residual hydrolyzer of formula agriculture |
| CN107022767A (en) * | 2017-05-10 | 2017-08-08 | 东北大学 | A kind of device that hydroxide is prepared for electrolytic metal chloride |
| CN107190274A (en) * | 2017-05-10 | 2017-09-22 | 东北大学 | A kind of method that nickel chloride electricity conversion directly prepares nickel hydroxide |
-
2017
- 2017-09-27 CN CN201710890667.7A patent/CN107674459A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN104120459A (en) * | 2014-08-06 | 2014-10-29 | 哈尔滨工业大学 | Preparation method of iron-based oxide colored pigment |
| CN104477950A (en) * | 2014-12-09 | 2015-04-01 | 四川大学 | Method for preparing high-purity alkaline magnesium carbonate and calcium carbonate by means of CO2 mineralization of dolomite |
| CN105542517A (en) * | 2016-01-14 | 2016-05-04 | 广西七色珠光材料股份有限公司 | White and interference-color matte flaky cored pigment and preparation method thereof |
| CN107022767A (en) * | 2017-05-10 | 2017-08-08 | 东北大学 | A kind of device that hydroxide is prepared for electrolytic metal chloride |
| CN107190274A (en) * | 2017-05-10 | 2017-09-22 | 东北大学 | A kind of method that nickel chloride electricity conversion directly prepares nickel hydroxide |
| CN107019141A (en) * | 2017-06-01 | 2017-08-08 | 稻思（上海）纳米科技有限公司 | One kind is thrown into the residual hydrolyzer of formula agriculture |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462197A (en) * | 2021-06-30 | 2021-10-01 | 常熟世名化工科技有限公司 | Preparation method of titanium dioxide aqueous dispersion, product and application thereof |
| CN113462197B (en) * | 2021-06-30 | 2022-08-09 | 常熟世名化工科技有限公司 | Preparation method of titanium dioxide aqueous dispersion, product and application thereof |
| CN115260796A (en) * | 2022-08-11 | 2022-11-01 | 福建坤彩材料科技股份有限公司 | Pearlescent pigment and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103952741A (en) | Aluminum alloy anodizing line treatment process | |
| CN102443825B (en) | High-concentration chromium sulfate-ammonium fluoride trivalent chromium electroplating solution and preparation method thereof | |
| TWI707067B (en) | Method and device for producing electroplating solution or electroplating replenishing solution for insoluble anode acid copper electroplating process | |
| CN107674459A (en) | The method that pigment hydrolyzes coating | |
| CN103590086A (en) | Nickel-free hole sealing agent for aluminum alloy and hole sealing treatment process of agent | |
| CN108193251B (en) | System and method for recovering nickel-tin salt coloring and medium-temperature hole sealing agent in aluminum processing | |
| CN105836792B (en) | A kind of production method of nano indium oxide | |
| CN108502985A (en) | A kind of the combined electrical chemical system and processing method of scale removal dechlorination | |
| TW201821654A (en) | Acid copper electroplating process using insoluble anode and equipment therefor | |
| CN103736994A (en) | Electroless nickel plating solution treatment method | |
| CN110644013B (en) | Indium oxide and preparation method of precursor thereof | |
| WO2023050565A1 (en) | Electrochemical hardness removal method for high-hardness, low-carbonate alkalinity coal gasification gray water | |
| CN112323084A (en) | Preparation method of nano indium oxide | |
| CN101525752B (en) | Clean production method for high-purity cobaltosic oxide powder | |
| CN103755080B (en) | Waste acid and wastewater reuse production process for hot galvanizing | |
| CN108545772A (en) | A kind of preparation method of colorant titanium dioxide additional hydrolyzing seed crystal | |
| CN105568341B (en) | A kind of tungsten oxide film and preparation method thereof | |
| CN105036423B (en) | Electrolytic treatment system of ship domestic sewage | |
| CN107761154A (en) | Application of the electrochemical process in pigment hydrolyzes coating | |
| CN108588723A (en) | A kind of regeneration cycle system and method for alkaline etching waste liquid for producing | |
| CN107675202A (en) | Pigment hydrolyzes coating reactor | |
| CN107630229A (en) | Pigment hydrolyzes coating reactor disturbed flow pipe | |
| JPH0432160B2 (en) | ||
| Lyu et al. | Efficient and clean manganese electrowinning in an anion-exchange membrane electrolyzer by pulse current electrodeposition method | |
| CN208667853U (en) | A kind of regeneration cycle system of alkaline etching waste liquid for producing |
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 |
Application publication date: 20180209 |
|
| RJ01 | Rejection of invention patent application after publication |