CN102888020B - Preparation method for brucite inorganic flame retardant - Google Patents
Preparation method for brucite inorganic flame retardant Download PDFInfo
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- CN102888020B CN102888020B CN201210356030.7A CN201210356030A CN102888020B CN 102888020 B CN102888020 B CN 102888020B CN 201210356030 A CN201210356030 A CN 201210356030A CN 102888020 B CN102888020 B CN 102888020B
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- brucite
- coupling agent
- flame retardant
- inorganic flame
- titanate coupling
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- 229910052599 brucite Inorganic materials 0.000 title claims abstract description 38
- 239000012796 inorganic flame retardant Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 23
- 230000004048 modification Effects 0.000 claims abstract description 23
- 239000007822 coupling agent Substances 0.000 claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 12
- 239000011707 mineral Substances 0.000 claims abstract description 12
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008117 stearic acid Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 4
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 230000003993 interaction Effects 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 239000003063 flame retardant Substances 0.000 description 7
- 235000010755 mineral Nutrition 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000012757 flame retardant agent Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical group [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005713 exacerbation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 102220043159 rs587780996 Human genes 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a preparation method for brucite inorganic flame retardant. The method comprises the following steps of: adding water into brucite mineral powder, mixing the brucite mineral powder and a dispersing agent, pulping in a superfine mill, grinding for a certain period of time, discharging pulp into a stirring barrel, and adding water to mix the pulp; adding KH-500 to modify by a wet method; and modifying through drying, wherein a coupling agent of organic titanate and stearic acid are added during drying. By the method, the chemical activity of the surface is improved by performing wet-method and dry-method compounded modification on brucite, the interaction between the brucite inorganic flame retardant and a basic resin can be enhanced, and the brucite inorganic flame retardant can be widely applied to the fields of low-smoke low-halogen content and smoke-free halogen-free plastic and the like.
Description
technical field:
The present invention relates to a kind of preparation method of brucite inorganic flame retardant, particularly relate to the preparation method of a kind of silane coupling agent wet method and titanate coupling agent, stearic acid dry laminating modification brucite inorganic flame retardant.
background technology:
The major ingredient of brucite is magnesium hydroxide, and it is the mineral that a kind of magnesium content of occurring in nature output is higher.It can be used as the fire retardant of polymer materials, rely on decomposition heat absorption and the water that discharges when applying and play fire retardation, there is nontoxicity, do not corrode processor, decompose after the advantage of magnesium oxide stable chemical nature that generates, therefore it is a kind of rare environment-friendly flame retardant agent, has become in fire retardant industry in recent years and has developed kind faster.But brucite is used as fire retardant exists again following shortcoming: brucite mineral are sheet or feather salt, specific surface area is large, and during the processing of high molecular material obtained, melting index is low, and material fluidity is poor, affects processing characteristics, surface irregularity. outward appearance is very poor; Surface polarity is too strong, and hydrophilic oleophobic, with the poor compatibility of organic materials; Flame retarding efficiency is low, must add in a large number and just can manifest flame retardant effect.Therefore above shortcoming makes the severe exacerbation such as mechanical property and processing characteristics of material.
Brucite makes fire retardant, and mineral surface modification is important step.Mineral surface modification is the bridgework between mineral and polymer, makes to form physical-chemical reaction between mineral and superpolymer, thus improves machining property and the mechanical property of matrix material, improves result of use.To the process of brucite mainly by carrying out dry method superfine grinding to brucite, obtained ultra-fine brucite powder, and then carry out powder surface modification with high-speed mixer interpolation tensio-active agent, micro mist is under the stirring of mixing machine paddle, rubbing effect, the reunion that gravitation between Preparation of Fine Powders impels generation strong, at this moment surface-modifying agent is added, the only properties-correcting agent at agglomerated particles Surface coating, and the small-particle in agglomerated particles does not obtain modification, namely modification is incomplete, and modified powder is no longer superfine powder.Brucite flame-retardant agent properties-correcting agent made by alone or double-purpose coupling agent is at present conventional method, but the product that such modification goes out is in matrix material, and mechanical property can't be met.
summary of the invention:
For solving the problem of brucite modified effect difference and modified application effect of products difference, carry out dry surface modification process when carrying out surface modification process and drying after the invention discloses a kind of brucite wet method super-fine, and use the collaborative composite modified technique of three kinds of different improved chemicals.
In wet method super-fine process, add dispersion agent, regulate the rheological property of ore pulp and the surface electrical behavior of ore particle, reduce the viscosity of ore pulp, promote the dispersion of particle; Add water after ultra-fine and size mixing to suitable modification concentration, then add KH-550(γ-aminopropyl triethoxysilane), powder is carried out surface modification; Again air stream drying is carried out to the ore pulp after wet-process modified, while drying, adopt titanate coupling agent, stearic acid composite modified.It is good that this wet-process modified and treatment process that the is composite modified integration of drying has modified effect, the flame retardant of magnesium hydroxide prepared can meet the application requiring of all kinds of macromolecular material such as PVC, EVA, PE, EPDM, particularly be applied in EVA, in extrusion, obvious discharging is fast, processing condition are good, and the product of making stretches rate greatly, and oxygen index is high, the composite products performance index of preparation are up to state standards, and have wide practical value.
A preparation method for brucite inorganic flame retardant, comprises the following steps:
(1) ultra-fine: the brucite breeze taking certainweight, add water and dispersion agent size mixing, pull an oar in Ultrafine Grinding, be ground to ore pulp median size D
50after=1 ~ 5 μm, blowing to agitation vat, add water size mixing to concentration be 30% ~ 50%(massfraction);
(2) wet-process modified: to join in agitation vat by the KH-550 silane coupling agent of brucite mineral grain weight amount 0.4% ~ 0.8%, stirring reaction 30 ~ 120 minutes, filters ore pulp after reacting completely;
(3) dry modification: add the titanate coupling agent of breeze weight 0.4% ~ 0.8% and the stearic acid of breeze weight 0.8% ~ 1.5% in the interval that dryer temperature is 100 ~ 180 DEG C.
Filter ore pulp in above-mentioned steps (2) after, then wash ore pulp, modified like this application effect of products is better, and major cause is that a small amount of residual dispersion agent has certain influence to the elongation of macromolecular material and specific conductivity.
Described titanate coupling agent is preferably titanate coupling agent TMC-TTS, titanate coupling agent HC-131, titanate coupling agent L-4.
Described dispersion agent is preferably Sodium hexametaphosphate 99, and it has excellent dispersiveness, easily washs, less on follow-up dry method modification impact.
In described brucite breeze, content of magnesia is greater than 65%.
Advantage of the present invention and effect are:
1, adopt KH-550 silane coupling agent, titanate coupling agent and stearic acid three kinds of composite modified brucites of properties-correcting agent, increase substantially the dispersiveness of brucite in macromolecule polymer material and consistency, improve the mechanical property of fire retardant material;
2, first under wet method condition, carry out modification, reaction is more abundant, then carries out modification to it while drying, achieves drying, modification integration, avoids the secondary agglomeration of common dry method modification;
3, wash the ore pulp after wet-process modified, modified like this application effect of products is better;
4, modified water magnesite product adds (every 100 parts of resins add 150 parts of modified water magnesites) in EVA to, and intensity is greater than 11 Mpa, and elongation at break is greater than 150%, and oxygen index is greater than 32s, and effect is remarkable.
embodiment:
Below in conjunction with embodiment, the present invention will be further described.
embodiment 1:take the 1250 order brucite breezes (content of MgO 65.8%) of 1000kg, add 1000kg water and 7kg Sodium hexametaphosphate 99 is sized mixing, pull an oar in Ultrafine Grinding, be ground to ore pulp median size D
50after=1.1 μm, blowing to agitation vat, add 2333kg water size mixing to concentration be 30%(massfraction); The KH-550 silane coupling agent adding 8kg joins in agitation vat, stirring reaction 120 minutes; Ore pulp is filtered, washs; Dry modification, the titanate coupling agent HC-131(Anhui Hong Chang additives for plastics company limited adding 8kg in the interval spraying that is 160 ~ 180 DEG C of pneumatic drier temperature produces) and the stearic acid of breeze weight 12kg.
embodiment 2: the 325 order brucite breezes (content of MgO 65.8%) taking 1000kg, add 667kg water and 5kg DC dispersion agent is sized mixing, pull an oar in Ultrafine Grinding, after being ground to ore pulp median size D50=4.8 μm, blowing to agitation vat, add 553kg water size mixing to concentration be 45%(massfraction); The KH-550 silane coupling agent adding 6kg joins in agitation vat, stirring reaction 120 minutes; Press filtration is carried out to ore pulp; Dry modification, the titanate coupling agent L-4(Chongqing Jia Shitai Chemical Co., Ltd. adding 4kg in the interval spraying that is 120 ~ 140 DEG C of pneumatic drier temperature produces) and the stearic acid of breeze weight 8kg.
embodiment 3:take the 1250 order brucite breezes (content of MgO 66.0%) of 1000kg, add 667kg water and 6kg Sodium hexametaphosphate 99 is sized mixing, pull an oar in Ultrafine Grinding, be ground to ore pulp median size D
50after=2.6 μm, blowing to agitation vat, add 833kg water size mixing to concentration be 40%(massfraction); The KH-550 silane coupling agent adding 4kg joins in agitation vat, stirring reaction 30 minutes; Ore pulp is filtered, washs; Dry modification, the green chemical industry auxiliary reagent factory of Tianzhang City of titanate coupling agent TMC-TTS(Anhui Province adding 6kg in the interval spraying that is 140 ~ 160 DEG C of pneumatic drier temperature produces) and the stearic acid of breeze weight 10kg.
embodiment 4:take the 1250 order brucite breezes (content of MgO 65.8%) of 1000kg, add 1000kg water and 7kg Sodium hexametaphosphate 99 is sized mixing, pull an oar in Ultrafine Grinding, be ground to ore pulp median size D
50after=2.1 μm, blowing to agitation vat, add 2333kg water size mixing to concentration be 30%(massfraction); The KH-550 silane coupling agent adding 6kg joins in agitation vat, stirring reaction 60 minutes; Ore pulp is filtered, washs; Dry modification, the titanate coupling agent L-4(Chongqing Jia Shitai Chemical Co., Ltd. adding 6kg in the interval spraying that is 100 ~ 120 DEG C of pneumatic drier temperature produces) and the stearic acid of breeze weight 10kg.
Be used for by the product of each embodiment (formula: resin 100 parts, composite modified brucite powder 150 parts) in EVA, the tensile strength of plastics Specifeca tion speeification, elongation at break, oxygen index, test result is in table 1.
(table 1)
Above-described embodiment that the present invention describes is only in order to technical scheme of the present invention is clearly described, and can not be interpreted as and make any restriction to the present invention.The present invention has known multiple alternative or distortion in the art, under the prerequisite not departing from essential meaning of the present invention, all falls into protection scope of the present invention.
Claims (3)
1. a preparation method for brucite inorganic flame retardant, is characterized in that, comprises the following steps:
(1) take the brucite breeze of certainweight, add water and dispersion agent size mixing, pull an oar in Ultrafine Grinding, be ground to ore pulp median size D
50after=1 ~ 5 μm, blowing to agitation vat, add water size mixing to concentration be 30% ~ 50%(massfraction);
(2) join in agitation vat by the KH-550 silane coupling agent of brucite mineral grain weight amount 0.4% ~ 0.8%, stirring reaction 30 ~ 120 minutes, filters ore pulp after reacting completely, washing;
(3) dry modification is carried out, the interval being 100 ~ 180 DEG C at dryer temperature adds titanate coupling agent and stearic acid, wherein titanate coupling agent is titanate coupling agent TMC-TTS, titanate coupling agent HC-131, titanate coupling agent L-4, titanate coupling agent consumption is 0.3% ~ 1.0% of brucite mineral grain weight amount, and stearic acid dosage is 0.8% ~ 1.5% of brucite mineral grain weight amount.
2. the preparation method of a kind of brucite inorganic flame retardant according to claim 1, is characterized in that, described dispersion agent is Sodium hexametaphosphate 99.
3. the preparation method of a kind of brucite inorganic flame retardant according to claim 1, is characterized in that, described brucite breeze content of magnesia is greater than 65%.
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| CN201210356030.7A CN102888020B (en) | 2012-09-24 | 2012-09-24 | Preparation method for brucite inorganic flame retardant |
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| CN201210356030.7A CN102888020B (en) | 2012-09-24 | 2012-09-24 | Preparation method for brucite inorganic flame retardant |
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| CN103663507A (en) * | 2013-09-16 | 2014-03-26 | 合肥中科阻燃新材料有限公司 | Method for preparing pure natural magnesium hydroxide flame retardant |
| CN103724663B (en) * | 2013-12-10 | 2016-01-13 | 辽宁亿龙矿业股份有限公司 | The preparation method of superfine active brucite composite modification material |
| CN105837856A (en) * | 2014-01-05 | 2016-08-10 | 陈旭 | Preparation method for inorganic fire retardant |
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| CN106220890A (en) * | 2016-07-26 | 2016-12-14 | 江苏西贝力新材料有限公司 | A kind of preparation method of superfine active basic magnesite fire-retardant filler |
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| CN114395274A (en) * | 2022-01-12 | 2022-04-26 | 江西广源化工有限责任公司 | Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material |
| CN115780035B (en) * | 2022-11-25 | 2023-09-29 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using horizontal wet ball mill |
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| US6376077B1 (en) * | 1998-04-10 | 2002-04-23 | Kyowa Chemical Industry Co., Ltd. | Process for the production of coupling agent-treated inorganic particles and use thereof |
| CN100384948C (en) * | 2006-06-09 | 2008-04-30 | 沈阳化工学院 | Composite modifier surface modified brucite powder preparation method |
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Owner name: XU MAOHANG Free format text: FORMER OWNER: CHEN XU Effective date: 20141218 |
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Inventor after: Xu Maohang Inventor before: Chen Xu |
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Free format text: CORRECT: INVENTOR; FROM: CHEN XU TO: XU MAOHANG Free format text: CORRECT: ADDRESS; FROM: 413101 YIYANG, HUNAN PROVINCE TO: 266000 QINGDAO, SHANDONG PROVINCE |
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Effective date of registration: 20141218 Address after: Licang District of Shandong province 266000 fo Lu Zheng Qingdao City No. 17 Applicant after: Xu Maohang Address before: 413101 Hunan city of Yiyang province Yuanjiang city Zhu Lian Xiang bamboo village two villagers Group Applicant before: Chen Xu |
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Inventor after: Cheng Fei Inventor before: Xu Maohang |
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Effective date of registration: 20170329 Address after: 528399 Guangdong province Foshan city Shunde District Daliang Xinyue Road No. 9 3 five sand block two factory (Shunde Industrial Park, industrial city) Patentee after: Shunde Guangdong with the way the new Mstar Technology Ltd Address before: Licang District of Shandong province 266000 fo Lu Zheng Qingdao City No. 17 Patentee before: Xu Maohang |