CN107502326A - A kind of secondary cross-linking carries liquid - Google Patents

A kind of secondary cross-linking carries liquid Download PDF

Info

Publication number
CN107502326A
CN107502326A CN201710784634.4A CN201710784634A CN107502326A CN 107502326 A CN107502326 A CN 107502326A CN 201710784634 A CN201710784634 A CN 201710784634A CN 107502326 A CN107502326 A CN 107502326A
Authority
CN
China
Prior art keywords
linking
secondary cross
crosslinking agent
carries liquid
liquid
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
CN201710784634.4A
Other languages
Chinese (zh)
Inventor
巫光胜
焦保雷
王瑞
钱真
吴文明
秦飞
何晓庆
甄恩龙
田亮
柏森
王敏健
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.)
China Petroleum and Chemical Corp
Original Assignee
China Petroleum and Chemical Corp
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 China Petroleum and Chemical Corp filed Critical China Petroleum and Chemical Corp
Priority to CN201710784634.4A priority Critical patent/CN107502326A/en
Publication of CN107502326A publication Critical patent/CN107502326A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/512Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5083Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a kind of secondary cross-linking to carry liquid, and by weight percentage, the secondary cross-linking, which carries liquid, to be included:0.08% 0.5% salt tolerant polymer, 0.07% 0.3% the first crosslinking agent, 0.1% 1.0% the second crosslinking agent, the water of 0.02% 0.07% oxygen scavenger and surplus.The secondary cross-linking of the present invention carries liquid and improves viscosity and stability, improves carrying capacity, high viscosity and long-time stability, which can be realized, carries particle to the purpose of oil deposit deep part, implement fixed point closure, improve water stream channel, to realize adjustment waterflood path, improve the purpose of water-flooding performance.

Description

A kind of secondary cross-linking carries liquid
Technical field
The invention belongs to oil-gas field development technical field, is specifically related to fractured-cavernous carbonate reservoir runner adjusting process A kind of secondary cross-linking carry liquid.
Background technology
The thickening that domestic and international fractured-cavernous carbonate reservoir runner adjusting process is formed also in starting stage, early stage at present There is significant limitation in what liquid took sand profile control technology and discarded slurry profile control technology, fail effectively solve carbonate rock fractured cave The unit water filling of type oil reservoir alter into problem.
For fracture-pore reservoir, matrix permeability is low (0.018 × 10-3um2), is flowed with Denudation pore, large-scale solution cavity etc. The extremely strong passage of kinetic force as preserving and flow unit, conventional profile control technology are difficult to be applicable, therefore propose using particle as The fracture-pore reservoir runner adjusting process of host, but how to realize that particle reaches specified location and implements closure steering target, also deposit In following problem:
(1) due to particle density itself, there is some difference with stratum water density, is difficult to realize and uniformly divides in the water of stratum Dissipate, because gravity difference, particle easily floats or settled in the earth formation, it is difficult to realizes that the target of stream is adjusted in deep.
(2) it is conventional at present to carry liquid:Temperature-resistant anti-salt energy be present in such as guanidine colloid system, thickening liquid system, polymeric system The problems such as power is limited, and the term of validity is short, under the conditions of high temperature (120 DEG C of >), high salt (> 200,000), easily degraded is realized, it is difficult to will Particle is carried to oil deposit deep part.
The content of the invention
The goal of the invention of the present invention is the defects of being directed to prior art, there is provided a kind of secondary cross-linking carries liquid.By weight Percentages, the secondary cross-linking, which carries liquid, to be included:0.08%-0.5% salt tolerant polymer, the first of 0.07%-0.3% are handed over Join agent, 0.1%-1.0% the second crosslinking agent, 0.02%-0.07% oxygen scavenger and the water of surplus.
Preferably, by weight percentage, the secondary cross-linking carries liquid and included:0.1%-0.3% salt tolerant polymer, 0.1%-0.2% the first crosslinking agent, 0.2%-0.8% the second crosslinking agent, 0.03%-0.05% oxygen scavenger and surplus Water.
Preferably, by weight percentage, the secondary cross-linking carries liquid and included:0.2% salt tolerant polymer, 0.15% The first crosslinking agent, 0.5% the second crosslinking agent, the water of 0.04% oxygen scavenger and surplus.
Preferably, the salt tolerant polymer is the hydrophobic association polyphosphazene polymer formed by polyacrylamide by modified poly Compound, molecular weight are 1800-2500 ten thousand.
Preferably, first crosslinking agent is chromium acetate and/or aluminium chloride.
Preferably, second crosslinking agent is acrylic acid and/or phenol.
Preferably, the oxygen scavenger is any one or more in sulphite, hydrazine and formaldehyde.
Preferably, the salt tolerant polymer first reacts to form a crosslinked at normal temperatures with first crosslinking agent System, after injecting stratum, a cross-linking system reacts to form secondary cross-linking body at the formation temperature with second crosslinking agent System.
Preferably, the viscosity of a cross-linking system is 150-300mPa.s.
Preferably, the viscosity of the secondary cross-linking system is 1800-2300mPa.s.
By adding salt tolerant polymer and the first crosslinking agent, increase the initial viscosity of system, ensure that carrying the initial of liquid takes Band ability;The second crosslinking agent is added, improves the viscosity and stability for carrying liquid, security system can preserve crosslinking steady in a long-term State, enhancing carry the long range carrying capacity of liquid, to realize the purpose that stream particle will be adjusted to be carried to oil deposit deep part, ensure and adjust stream Particle can reach design object, ensure construction effect.
Embodiment
In order to be fully understood by the purpose of the present invention, feature and effect, by following embodiments, the present invention is made detailed Describe in detail bright.For the process of the present invention in addition to the description below, remaining uses the conventional method or device of this area.Following nouns Term is unless otherwise stated, be respectively provided with the implication that those skilled in the art are generally understood that.
Limited for conventional carrying liquid carrying capacity, the term of validity is short, it is difficult to realizes the problem of deep carries, inventor's research The system for carrying liquid carrying capacity is improved, due to adjusting density variation between stream particle and stratum water and fracture-pore reservoir reservoir to stitch Hole developmental state, particle easily float or settled, and the system improves the viscosity and stability for carrying liquid, improve and carry taking for liquid Band ability, the high viscosity and long-time stability of system, which can be realized, carries particle to the purpose of oil deposit deep part, implements fixed point envelope It is stifled, improve water stream channel, to realize adjustment waterflood path, improve the purpose of water-flooding performance.
Specifically, the invention provides a kind of secondary cross-linking to carry liquid, and by weight percentage, the secondary cross-linking carries Liquid includes:0.08%-0.5% salt tolerant polymer, 0.07%-0.3% the first crosslinking agent, the second of 0.1%-1.0% are handed over Join agent, 0.02%-0.07% oxygen scavenger and the water of surplus;Preferably, the secondary cross-linking carries liquid and included:0.1%- 0.3% salt tolerant polymer, 0.1%-0.2% the first crosslinking agent, 0.2%-0.8% the second crosslinking agent, 0.03%- 0.05% oxygen scavenger and the water of surplus;It is highly preferred that 0.2% salt tolerant polymer, 0.15% the first crosslinking agent, 0.5% The second crosslinking agent, the water of 0.04% oxygen scavenger and surplus.
Wherein, the salt tolerant polymer is the hydrophobic association high molecular polymerization formed by polyacrylamide by modified poly Thing, molecular weight are 1800-2500 ten thousand.Polyacrylamide (PAM) be by acrylamide (AM) monomer through free radical polymerization and Into water-soluble linear high molecular polymer, in the present invention, by the course of the polymerization process to polymer molecular chain introduce it is hydrophobic Group is realized to the hydrophobically modified of polymer so as to obtain hydrophobic association high molecular polymer.In one embodiment, pass through By N, N '-dimethyl acryloyl-oxy butyl alkyl bromination ammonium (DMABA) introduces polymer macromolecule chain, so as to realize to polypropylene The hydrophobically modified of acid amides.Specifically, for example, with AIBA (azo diisobutyl amidine hydrochloride) for initiator, initiation temperature 10- 15 DEG C, according to concentration of the DMABA in reaction system be 20-30wt% prepare hydrophobically modified polyacrylamide (HMPAM), with Make the salt tolerant polymer of the present invention.
Wherein, the first crosslinking agent is chromium acetate and/or aluminium chloride, can pass through conventional acquisition purchased in market.
Wherein, the second crosslinking agent is acrylic acid and/or phenol, can pass through conventional acquisition purchased in market.
Wherein, oxygen scavenger is any one in sulphite (such as sodium sulfite, potassium sulfite etc.), hydrazine and formaldehyde Or it is a variety of, conventional acquisition purchased in market can be passed through.
Wherein, the water can be stratum water.
Salt tolerant polymer, the first crosslinking agent, the second crosslinking agent, oxygen scavenger and stratum water are well mixed i.e. according to aforementioned proportion It can obtain the carrying liquid of the present invention.
The density of the carrying liquid of the present invention is 0.90-1.30g/cm3(preferably 1.10-1.20g/cm3, more preferably 1.14g/ cm3), it is suitably adapted for the same fractured-vuggy reservoir of stratum water density.
Above-mentioned each component has synergy afterwards according to aforementioned proportion combination.Specifically, salt tolerant polymer and first is handed over 0.5-2 hours reacts in connection agent under normal temperature (such as 20-26 DEG C) can form a cross-linking system, can increase and carry initially gluing for liquid (viscosity increases to 150-300mPa.s, preferably 240-300mPa.s) and carrying capacity are spent, improves temperature-resistant anti-salt ability.Treating will After carrying liquid injection stratum, (such as 110-130 DEG C) reacts 8-20 at the formation temperature for a cross-linking system and the second crosslinking agent Hour can form secondary cross-linking system, and viscosity can continue to increase to 2000mPa.s or so (such as 1800-2300mPa.s), enter one Step improves the carrying capacity for carrying liquid, while secondary cross-linking system can keep not breaking glue in 7-15 days, it is ensured that system has There is sufficiently strong carrying capacity, to realize that the fixed point for adjusting stream particle carries, realizing improves waterflood path, improves water-flooding performance Purpose.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to described reality Apply among a scope.The experimental method of unreceipted actual conditions in the following example, conventionally and condition.Following implementation The raw material used in example is conventional acquisition purchased in market.
Embodiment 1 prepares secondary cross-linking and carries liquid sample 1#
Hydrophobically modified polyacrylamide 0.2g is weighed, the first crosslinking agent chromium acetate 0.15g, weighs the second crosslinking agent acrylic acid 0.5g, under the conditions of 1000r/min high-speed stirreds, once add (density 1.14g/cm in 1000ml stratum water3), stirring 30min, uniform solution is configured to, obtains secondary cross-linking and carry liquid sample 1#.
Embodiment 2 prepares secondary cross-linking and carries liquid sample 2#
Hydrophobically modified polyacrylamide 0.3g is weighed, the first crosslinking agent aluminium chloride 0.2g, weighs the second crosslinking agent phenol 0.6g, under the conditions of 1000r/min high-speed stirreds, once add (density 1.14g/cm in 1000ml stratum water3), stirring 30min, uniform solution is configured to, determines a crosslinked viscosity;Crosslinked fluid is put into 120 DEG C of baking ovens, obtained secondary Crosslinking carries liquid sample 2#.
Embodiment 3 determines the gelling strength and gelation time of the secondary cross-linking liquid of Examples 1 and 2.
Gelling strength and gelation time assay method are as follows:
Example 1 and the secondary cross-linking of embodiment 2 carry the viscosity after liquor 100ml measure is once crosslinked respectively, Then add in cillin bottle (100ml) and seal, be put into 120 DEG C of baking oven and heat plastic and timing, every 1 hour observation plastic feelings Condition, when the quick retrogradation of water shutoff agent, per 30min HAKKE RS150 high temperature rheometers, in shear rate 1.5S1Lower measure is frozen Glue intensity, the time when gel strength reaches maximum are gelation time, and the intensity when gel strength is stable is frozen glue Intensity, specific measurement result are as shown in table 1.
Table 1
Embodiment 4-8
The composition that embodiment 4-8 secondary cross-linking carries liquid is as shown in table 2.
Table 2
Effete test embodiment
The carrying liquid of the present invention is configured using stratum water, is handed over by adding salt tolerant polymer and first in carrying liquid in particle Join agent, increase the initial viscosity of system, ensure the initial carrying capacity for carrying liquid;The second crosslinking agent is added, improves and carries liquid Viscosity and stability, the cross-linked state that security system can maintain a long-term stability, enhancing carry the long range carrying capacity of liquid, with The purpose that stream particle will be adjusted to be carried to oil deposit deep part is realized, ensures and adjusts stream particle to reach design object, ensure construction effect.
The secondary cross-linking solution and 0.2% each 100L of guanidine glue of embodiment 1 are configured, is adjusted in flat plate model is visualized The carrying migration experiment of particle is flowed, contrast secondary cross-linking carries the carrying migration ability of liquid and guanidine glue.Experimental temperature is room temperature, Flat board long 4m, high 0.6m, wide 6mm, migration velocity 0.4m/s are visualized, experiment shows that secondary cross-linking carries liquid and under the low speed can It is enough that stream particle will be adjusted to carry out flat plate model completely, and 0.2% guanidine glue adjusts stream particle can rapid subsidence under 0.4m/s speed In flat plate model bottom, illustrate to carry liquid energy using secondary cross-linking and greatly enhance to exchange to flow particle carrying migration distance.
The present invention is hereinbefore disclosed with preferred embodiment, but it should be understood by those skilled in the art that, these Embodiment is only used for describing the present invention, and should not be construed as limiting the scope of the present invention.It should be noted that every implement with these Example equivalent change and displacement, all should be set to be covered by scope of the presently claimed invention.Therefore, protection scope of the present invention It should be defined by the scope defined in claims.

Claims (10)

1. a kind of secondary cross-linking carries liquid, it is characterised in that by weight percentage, the secondary cross-linking, which carries liquid, to be included: 0.08%-0.5% salt tolerant polymer, 0.07%-0.3% the first crosslinking agent, 0.1%-1.0% the second crosslinking agent, 0.02%-0.07% oxygen scavenger and the water of surplus.
2. secondary cross-linking according to claim 1 carries liquid, it is characterised in that by weight percentage, the secondary friendship Connection, which carries liquid, to be included:0.1%-0.3% salt tolerant polymer, 0.1%-0.2% the first crosslinking agent, the of 0.2%-0.8% The water of two crosslinking agents, 0.03%-0.05% oxygen scavenger and surplus.
3. secondary cross-linking according to claim 1 or 2 carries liquid, it is characterised in that by weight percentage, described secondary Crosslinking, which carries liquid, to be included:0.2% salt tolerant polymer, 0.15% the first crosslinking agent, 0.5% the second crosslinking agent, 0.04% Oxygen scavenger and surplus water.
4. secondary cross-linking according to claim any one of 1-3 carries liquid, it is characterised in that the salt tolerant polymer be by The hydrophobic association high molecular polymer that polyacrylamide is formed by modified poly, molecular weight are 1800-2500 ten thousand.
5. the secondary cross-linking according to claim any one of 1-4 carries liquid, it is characterised in that first crosslinking agent is second Sour chromium and/or aluminium chloride.
6. the secondary cross-linking according to claim any one of 1-5 carries liquid, it is characterised in that second crosslinking agent is third Olefin(e) acid and/or phenol.
7. the secondary cross-linking according to claim any one of 1-6 carries liquid, it is characterised in that the oxygen scavenger is sulfurous acid Any one or more in salt, hydrazine and formaldehyde.
8. the secondary cross-linking according to claim any one of 1-7 carries liquid, it is characterised in that the salt tolerant polymer and institute The first crosslinking agent is stated first to react to form a cross-linking system at normal temperatures, inject stratum after, a cross-linking system with Second crosslinking agent reacts to form secondary cross-linking system at the formation temperature.
9. secondary cross-linking according to claim 8 carries liquid, it is characterised in that the viscosity of a cross-linking system is 150-300mPa.s。
10. secondary cross-linking according to claim 8 carries liquid, it is characterised in that the viscosity of the secondary cross-linking system is 1800-2300mPa.s。
CN201710784634.4A 2017-09-04 2017-09-04 A kind of secondary cross-linking carries liquid Pending CN107502326A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710784634.4A CN107502326A (en) 2017-09-04 2017-09-04 A kind of secondary cross-linking carries liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710784634.4A CN107502326A (en) 2017-09-04 2017-09-04 A kind of secondary cross-linking carries liquid

Publications (1)

Publication Number Publication Date
CN107502326A true CN107502326A (en) 2017-12-22

Family

ID=60695614

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710784634.4A Pending CN107502326A (en) 2017-09-04 2017-09-04 A kind of secondary cross-linking carries liquid

Country Status (1)

Country Link
CN (1) CN107502326A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965088A (en) * 2012-11-20 2013-03-13 西南石油大学 Environment-friendly crosslinking and gelling retarding profile control agent and preparation method thereof
CN103468230A (en) * 2013-08-12 2013-12-25 中国石油天然气股份有限公司 Secondary cross-linking profile control and flooding agent and preparation method and application thereof
CN104357032A (en) * 2014-10-13 2015-02-18 中国石油化工股份有限公司 High-temperature resistant secondary cross-linked gel profile control agent and preparation method thereof
CN104987857A (en) * 2015-06-25 2015-10-21 中国石油天然气股份有限公司 High-salt-resistant self-tackifying hydrophobically associating polymer gel plugging agent and preparation method thereof
CN106047330A (en) * 2016-06-15 2016-10-26 中国海洋石油总公司 Secondarily crosslinked aqueous gel crosslinking agent and preparation method and application thereof
CN106479463A (en) * 2016-09-19 2017-03-08 中国石油大学(华东) Retarded crosslinking high intensity frozen glue profile-controlling and plugging agent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965088A (en) * 2012-11-20 2013-03-13 西南石油大学 Environment-friendly crosslinking and gelling retarding profile control agent and preparation method thereof
CN103468230A (en) * 2013-08-12 2013-12-25 中国石油天然气股份有限公司 Secondary cross-linking profile control and flooding agent and preparation method and application thereof
CN104357032A (en) * 2014-10-13 2015-02-18 中国石油化工股份有限公司 High-temperature resistant secondary cross-linked gel profile control agent and preparation method thereof
CN104987857A (en) * 2015-06-25 2015-10-21 中国石油天然气股份有限公司 High-salt-resistant self-tackifying hydrophobically associating polymer gel plugging agent and preparation method thereof
CN106047330A (en) * 2016-06-15 2016-10-26 中国海洋石油总公司 Secondarily crosslinked aqueous gel crosslinking agent and preparation method and application thereof
CN106479463A (en) * 2016-09-19 2017-03-08 中国石油大学(华东) Retarded crosslinking high intensity frozen glue profile-controlling and plugging agent

Similar Documents

Publication Publication Date Title
CN104612639B (en) Process of deep profile control over low-permeability oil reservoir
CN102952533B (en) Composite cross-linked polymer weak gel oil displacement agent and preparation method thereof
CN109369848A (en) A kind of functional form temperature-resistant anti-salt plugging agent and preparation method thereof
CN103216211B (en) Profile control method for fractured reservoir
CN102603968A (en) High molecular polymer water absorbing material for well drilling leak stoppage
CN102453473B (en) Organogel blocking agent for water blocking and profile control, and preparation method and application thereof
CN106883357A (en) A kind of pre-crosslinked gel delays swollen microballoon profile control agent and its production and use
CN112409611B (en) Mussel bionic gel composition, self-repairing gel and plugging agent as well as preparation method and application of self-repairing gel and plugging agent
CN104479653A (en) Retarding-swelling salt-tolerant high-viscoelasticity particles with interpenetrating network structure and preparation method thereof
CN105925255B (en) High-temperature profile control temporary plugging agent and preparation method and application thereof
CN110129013B (en) Organic-inorganic composite gel plugging agent and preparation method and application thereof
CN109385259B (en) AM-AMPS-NVP terpolymer-PR temperature-resistant profile control agent and preparation method and application thereof
CN101724384A (en) Preparation method of high-strength elastic slow-expansion water-absorbing particle diverting agent
CN107502325A (en) Preparation method and application of high-temperature-resistant high-salt profile control and flooding agent
CN106590559B (en) The nano combined frozen glue of heavy oil thermal recovery fleeing proof
CN109735315A (en) A kind of environment-friendly type oil recovery delay crosslinking profile control agent and preparation method and purposes
CN106008803A (en) High temperature resistant cross-linked acid thickening agent and preparation method thereof
CN105368423A (en) Chromium-free composite resin gel-type profile control agent for oil exploitation and preparation method and application thereof
CN105820804B (en) Hypersalinity-resistant oil reservoir deep liquid flow diversion chemical agent and preparation method and application thereof
CN105112034B (en) High-temperature-resistant gel diverting agent and preparation method and application thereof
CN108728068A (en) A kind of preparation method of the underground polymerization water shutoff agent of suitable high-temperature oil reservoir
CN104710568A (en) Preparation method of retarding swelling anti-salt viscoelastic particle profile control agent
CN102603969B (en) A kind of cementing properties GEL USED FOR PLUGGING WELL LOST CIRCULATION and preparation method thereof
CN102408518B (en) Microcrosslinking polymer for oil displacement and preparation method thereof
CN105669896B (en) Thermosensitive copolymer gel profile control water shutoff agent and preparation method and application thereof

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: 20171222