CN204643856U - A kind of equipment of preparing silane with trichlorosilane - Google Patents

A kind of equipment of preparing silane with trichlorosilane Download PDF

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Publication number
CN204643856U
CN204643856U CN201520320211.3U CN201520320211U CN204643856U CN 204643856 U CN204643856 U CN 204643856U CN 201520320211 U CN201520320211 U CN 201520320211U CN 204643856 U CN204643856 U CN 204643856U
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cylindrical shell
hypomere
liquid
stage casing
epimere
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柴新刚
刘明亮
梁正
张艾民
马秀艳
胡丽娟
陈雷
杨欢欢
王采蓓
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Henan silane science and technology development Limited by Share Ltd
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SEDIN NINGBO ENGINEERING Co Ltd
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Abstract

The utility model discloses a kind of equipment of preparing silane with trichlorosilane, feature comprises diameter from bottom to top to successively decrease successively and hypomere cylindrical shell spaced apart from each other, stage casing cylindrical shell and epimere cylindrical shell, hypomere cylinder top is provided with hypomere overhead-liquid entrance and the outlet of hypomere top gas, extend the center in hypomere cylindrical shell in hypomere overhead-liquid entrance and connect charging distribution pipe, the below of charging distribution pipe is provided with a hypomere catalyst layer, two-layer hypomere packing layer is provided with below lower section catalyst layer, cylindrical shell top, stage casing is provided with stage casing overhead-liquid entrance and the outlet of stage casing top gas, stage casing liquid distributor is provided with below the overhead-liquid entrance of stage casing cylindrical shell inherent stage casing, stage casing catalyst layer is provided with below the liquid distributor of stage casing, epimere cylindrical shell top is provided with epimere overhead-liquid entrance, top end socket is provided with the outlet of epimere top gas, advantage uses support equipment few, contain two silane reaction devices and two rectifying tower.

Description

A kind of equipment of preparing silane with trichlorosilane
Technical field
The utility model belongs to chemical field, especially relates to a kind of equipment of preparing silane with trichlorosilane.
Background technology
Silane, as a kind of gas source providing silicon components, is the intermediate product of the granular high purity silicon of scale operation unique in the world so far.Can be used for manufacturing high-purity polycrystalline silicon, silicon single crystal, microcrystal silicon, non-crystalline silicon, various metal silicide.Because its high purity finely controls with realizing, become the important special gas that other silicon sources many cannot replace.
Chlorosilane hydrogenation and secondary disproportionation reaction prepare the method that silane is production silane important in the world at present.The method is with hydrogen at high temperature direct-reduction chlorosilane generation trichlorosilane, carries out secondary disproportionation reaction subsequently and prepares silane.Secondary disproportionation reaction will have been come by two rectifying tower and two reactors, and each rectifying tower and reactor have supporting heat-exchange equipment and surge tank.Therefore have that the technological process of production is long, equipment is various, occupation of land is large, invest high shortcoming.
Summary of the invention
It is few that technical problem to be solved in the utility model is to provide a kind of support equipment that uses, and contains the equipment of the preparing silane with trichlorosilane of silane reaction and rectifying.
The utility model solves the problems of the technologies described above adopted technical scheme: a kind of equipment of preparing silane with trichlorosilane, comprise the hypomere cylindrical shell that diameter from bottom to top successively decreases successively, stage casing cylindrical shell, epimere cylindrical shell, described hypomere cylindrical shell is connected by lower conical shell one with described stage casing cylindrical shell, described stage casing cylindrical shell is connected by upper conical shell one with described epimere cylindrical shell, described hypomere cylindrical shell and described stage casing cylindrical shell are separated by spherical lower cover and described lower cover is positioned at the below of described lower conical shell, described stage casing cylindrical shell and described epimere cylindrical shell are separated by spherical upper cover and described upper cover is positioned at the below of described upper conical shell, the bottom of described hypomere cylindrical shell is provided with bottom bulkhead, the top of described epimere cylindrical shell is provided with top end socket,
The barrel top of described hypomere cylindrical shell is provided with hypomere overhead-liquid entrance and the outlet of hypomere top gas, extend the center in described hypomere cylindrical shell in described hypomere overhead-liquid entrance and connect the charging distribution pipe being positioned at described hypomere cylindrical shell, the below of the described charging distribution pipe described in hypomere cylindrical shell inherence is provided with a hypomere catalyst layer, two-layer hypomere packing layer is provided with below the described lower section catalyst layer described in hypomere cylindrical shell inherence, hypomere liquid distributor is provided with between described charging distribution pipe and described lower section catalyst layer, liquid collecting redistributor is respectively arranged with between hypomere packing layer between described lower section catalyst layer and the hypomere packing layer described in upper strata and described in upper strata and the hypomere packing layer described in lower floor, described bottom bulkhead is provided with hypomere bottom liquid outlet,
The barrel top of described stage casing cylindrical shell is provided with stage casing overhead-liquid entrance and the outlet of stage casing top gas, the center in described stage casing cylindrical shell is extended in described stage casing overhead-liquid entrance, stage casing liquid distributor is provided with below the described stage casing overhead-liquid entrance described in cylindrical shell inherence, stage casing, stage casing catalyst layer is provided with below the described stage casing liquid distributor described in cylindrical shell inherence, stage casing, described lower conical shell is provided with stage casing bottom gas inlet, and the bottom of described lower conical shell is provided with stage casing bottom liquid outlet;
The barrel top of described epimere cylindrical shell is provided with epimere overhead-liquid entrance, the center in described epimere cylindrical shell is extended in described epimere overhead-liquid entrance, the described epimere overhead-liquid entrance top described in epimere cylindrical shell inherence is provided with scum dredger, epimere liquid distributor is provided with below the described epimere overhead-liquid entrance described in epimere cylindrical shell inherence, epimere packing layer is provided with below the described epimere liquid distributor described in epimere cylindrical shell inherence, described upper conical shell is provided with epimere bottom gas inlet, the bottom of described upper conical shell is provided with epimere bottom liquid outlet, described top end socket is provided with the outlet of epimere top gas.
Described liquid collecting redistributor comprises several inverted L shape liquid collecting plates, liquid cylinder, liquid trap ring, downtake, distribution piping, distribution showerhead, one-level distribution trough and secondary distribution groove, described inverted L shape liquid collecting plate is positioned at the top of described liquid cylinder, described inverted L shape liquid collecting plate is symmetrically distributed in the both sides of described liquid cylinder and the described outward-dipping setting of inverted L shape liquid collecting plate, described liquid cylinder is fixed on described liquid trap ring, the periphery of described liquid trap ring is fixed on the inwall of described hypomere cylindrical shell, described liquid trap ring, intercepting basin is formed between described liquid cylinder and described hypomere cylindrical shell three, described liquid cylinder is communicated with described distribution piping respectively by described downtake with described intercepting basin, the lower surface of described distribution piping is evenly equipped with several distribution showerhead, the below of described distribution showerhead is provided with one-level distribution trough, the lower surface of described one-level distribution trough is evenly equipped with several secondary distribution grooves.Liquid collecting redistributor is made up of upper and lower two portions, top is used for liquid bulk to collect, bottom is used for liquid to carry out uniformly distributing, liquid is fallen on L-type liquid collecting plate, flow in the ring groove that liquid cylinder and liquid trap ring and hypomere cylindrical shell formed from liquid collecting plate two ends, liquid flows in distribution piping from downtake again, has flow in one-level distribution trough by the distribution showerhead on distribution piping, liquid flows in secondary distribution groove in one-level distribution trough, reaches the effect of evenly distributing liquid.
The diameter of described hypomere cylindrical shell is 1 ~ 3 meter, the diameter of described stage casing cylindrical shell is 0.6 ~ 1.5 meter, the diameter of described epimere cylindrical shell is 0.3 ~ 1 meter, the height of described lower section catalyst layer is 1 ~ 4 meter, the height of described hypomere packing layer is 1 ~ 4 meter, the height of described stage casing catalyst layer is 1 ~ 4 meter, and the height of described epimere packing layer is 1 ~ 4 meter.
Compared with prior art, the utility model has the advantage of: the utility model makes public for the first time a kind of equipment of preparing silane with trichlorosilane, use the equipment that support equipment is few, contain silane reaction and rectifying, this equipment contains the function that two reactors mentioning in technical background and two rectifying tower have, there is structure simple, reaction efficiency is high, less investment, takes up an area little advantage.The silane purity utilizing these apparatus and method to produce reaches 99.99999%.
Accompanying drawing explanation
Fig. 1 is the structural representation of the equipment of the utility model preparing silane with trichlorosilane;
Fig. 2 is the structural representation of the utility model liquid collecting redistributor.
Embodiment
Below in conjunction with accompanying drawing embodiment, the utility model is described in further detail.
Specific embodiment one
A kind of equipment of preparing silane with trichlorosilane, as shown in Figure 1, comprise the hypomere cylindrical shell 3 that diameter from bottom to top successively decreases successively, stage casing cylindrical shell 11, epimere cylindrical shell 16, hypomere cylindrical shell 3 is connected by lower conical shell 10 one with stage casing cylindrical shell 11, stage casing cylindrical shell 11 is connected by upper conical shell 14 one with epimere cylindrical shell 16, hypomere cylindrical shell 3 and stage casing cylindrical shell 11 are separated by spherical lower cover 9 and lower cover 9 is positioned at the below of lower conical shell 10, stage casing cylindrical shell 11 and epimere cylindrical shell 16 are separated by spherical upper cover 13 and upper cover 13 is positioned at the below of upper conical shell 14, the bottom of hypomere cylindrical shell 3 is provided with bottom bulkhead 2, the top of epimere cylindrical shell 16 is provided with top end socket 18,
The barrel top of hypomere cylindrical shell 3 is provided with hypomere overhead-liquid entrance 29 and hypomere top gas outlet 8, extend the center in hypomere cylindrical shell 3 in hypomere overhead-liquid entrance 29 and connect the charging distribution pipe 30 being positioned at hypomere cylindrical shell 3, the below of the inherent charging distribution pipe 30 of hypomere cylindrical shell 3 is provided with a hypomere catalyst layer 6, two-layer hypomere packing layer 4 is provided with below hypomere cylindrical shell 3 inherent lower section catalyst layer 6, hypomere liquid distributor 7 is provided with between charging distribution pipe 30 and lower section catalyst layer 6, liquid collecting redistributor 5 is respectively arranged with between lower section catalyst layer 6 and upper strata hypomere packing layer 4 and between upper strata hypomere packing layer 4 and lower floor's hypomere packing layer 4, bottom bulkhead 2 is provided with hypomere bottom liquid outlet 1,
The barrel top of stage casing cylindrical shell 11 is provided with stage casing overhead-liquid entrance 24 and stage casing top gas outlet 12, the center in stage casing cylindrical shell 11 is extended in stage casing overhead-liquid entrance 24, stage casing liquid distributor 25 is provided with below stage casing cylindrical shell 11 inherent stage casing overhead-liquid entrance 24, stage casing catalyst layer 26 is provided with below stage casing cylindrical shell 11 inherent stage casing liquid distributor 25, lower conical shell 10 is provided with stage casing bottom gas inlet 27, and the bottom of lower conical shell 10 is provided with stage casing bottom liquid outlet 28;
The barrel top of epimere cylindrical shell 16 is provided with epimere overhead-liquid entrance 20, the center in epimere cylindrical shell 16 is extended in epimere overhead-liquid entrance 20, scum dredger 17 is provided with above epimere cylindrical shell 16 inherent epimere overhead-liquid entrance 20, epimere liquid distributor 21 is provided with below epimere cylindrical shell 16 inherent epimere overhead-liquid entrance 20, epimere packing layer 15 is provided with below the inherent epimere liquid distributor 21 of epimere cylindrical shell 16, upper conical shell 14 is provided with epimere bottom gas inlet 22, the bottom of upper conical shell 14 is provided with epimere bottom liquid outlet 23, top end socket 18 is provided with epimere top gas outlet 19.
In this particular embodiment, as shown in Figure 2, liquid collecting redistributor 5 comprises several inverted L shape liquid collecting plates 59, liquid cylinder 58, liquid trap ring 56, downtake 55, distribution piping 54, distribution showerhead 53, one-level distribution trough 52 and secondary distribution groove 51, inverted L shape liquid collecting plate 59 is positioned at the top of liquid cylinder 58, inverted L shape liquid collecting plate 59 is symmetrically distributed in the both sides of liquid cylinder 58 and the outward-dipping setting of inverted L shape liquid collecting plate 59, liquid cylinder 58 is fixed on liquid trap ring 56, the periphery of liquid trap ring 56 is fixed on the inwall of hypomere cylindrical shell 3, liquid trap ring 56, intercepting basin 57 is formed between liquid cylinder 58 and hypomere cylindrical shell 3 three, liquid cylinder 58 is communicated with distribution piping 54 respectively by downtake 55 with intercepting basin 57, the lower surface of distribution piping 54 is evenly equipped with several distribution showerhead 53, the below of distribution showerhead 53 is provided with one-level distribution trough 52, the lower surface of one-level distribution trough 52 is evenly equipped with several secondary distribution grooves 51.Liquid collecting redistributor 5 is made up of upper and lower two portions, top is used for liquid bulk to collect, bottom is used for liquid to carry out uniformly distributing, liquid is fallen on L-type liquid collecting plate, flow to from liquid collecting plate two ends in the ring groove that liquid cylinder 58 and liquid trap ring 56 and hypomere cylindrical shell 3 formed, liquid flows in distribution piping 54 from downtake 55 again, flow in one-level distribution trough 52 by the distribution showerhead 53 on distribution piping 54, liquid flows in secondary distribution groove 51 in one-level distribution trough 52, reaches the effect of evenly distributing liquid.
In this particular embodiment, the diameter of hypomere cylindrical shell 3 is 1 ~ 3 meter, the diameter of stage casing cylindrical shell 11 is 0.6 ~ 1.5 meter, the diameter of epimere cylindrical shell 16 is 0.3 ~ 1 meter, the height of lower section catalyst layer 6 is 1 ~ 4 meter, the height of hypomere packing layer 4 is 1 ~ 4 meter, and the height of stage casing catalyst layer 26 is 1 ~ 4 meter, and the height of epimere packing layer 15 is 1 ~ 4 meter.Three sections of barrel diameters can adjust according to the output of silane.Above-mentioned all parts all adopt ultra-low carbon austenitic stainless steel material to make, and adopt ultra-low carbon austenitic stainless steel as material, effectively can reduce the pollution to product.
Specific embodiment two
Utilize the equipment of the preparing silane with trichlorosilane described in above-mentioned specific embodiment 1 to prepare a method for silane, as shown in Figure 1, comprise the following steps:
(1) trichlorosilane liquid is sent in hypomere cylindrical shell 3 from hypomere overhead-liquid entrance 29, be evenly distributed on lower section catalyst layer 6 by charging distribution pipe 30 and hypomere liquid distributor 7 successively, lower section catalyst layer 6 generates silane, silicon tetrachloride and intermediate product after reaction, silane, silicon tetrachloride and intermediate product carry out effect of mass transmitting successively on two-layer hypomere packing layer 4, silicon tetrachloride is discharged from hypomere bottom liquid outlet 1, and silane and intermediate product are discharged from hypomere top gas outlet 8;
(2) by after silane and intermediate product cooling, partial intermediate is back in hypomere cylindrical shell 3 from hypomere overhead-liquid entrance 29, silane gas with partial intermediate is sent in stage casing cylindrical shell 11 from stage casing bottom gas inlet 27, on stage casing catalyst layer 26, intermediate product is continued to react with the liquid entered by stage casing overhead-liquid entrance 24 and generates silane, silane gas with a small amount of intermediate product and impurity is discharged from stage casing top gas outlet 12, liquid with intermediate product is discharged from stage casing bottom liquid outlet 28, be back in hypomere cylindrical shell 3 by hypomere overhead-liquid entrance 29,
(3) after the silane gas with a small amount of intermediate product and impurity being cooled further, intermediate product is flow back in stage casing cylindrical shell 11 from stage casing overhead-liquid entrance 24, silane gas with few partial intermediate and impurity is sent in epimere cylindrical shell 16 from epimere bottom gas inlet 22, epimere packing layer 15 carries out effect of mass transmitting with the liquid entered from epimere overhead-liquid entrance 20, the silane gas of removing intermediate product is discharged from epimere top gas outlet 19, liquid with intermediate product is discharged from epimere bottom liquid outlet 23, be back in stage casing cylindrical shell 11 by stage casing overhead-liquid entrance 24, by the silane gas from epimere top gas outlet 19 discharge after condensation, small part is back to epimere cylindrical shell 16 from epimere overhead-liquid entrance 20, major part enters subsequent handling and purifies further.
In this particular embodiment, liquid collecting redistributor 5 is respectively arranged with between lower section catalyst layer 6 and upper strata hypomere packing layer 4 and between upper strata hypomere packing layer 4 and lower floor's hypomere packing layer 4, stage casing liquid distributor 25 is provided with below stage casing cylindrical shell 11 inherent stage casing overhead-liquid entrance 24, be provided with epimere liquid distributor 21 below epimere cylindrical shell 16 inherent epimere overhead-liquid entrance 20, above epimere cylindrical shell 16 inherent epimere overhead-liquid entrance 20, be provided with scum dredger 17.
In this particular embodiment, as shown in Figure 2, liquid collecting redistributor 5 comprises several inverted L shape liquid collecting plates 59, liquid cylinder 58, liquid trap ring 56, downtake 55, distribution piping 54, distribution showerhead 53, one-level distribution trough 52 and secondary distribution groove 51, inverted L shape liquid collecting plate 59 is positioned at the top of liquid cylinder 58, inverted L shape liquid collecting plate 59 is symmetrically distributed in the both sides of liquid cylinder 58 and the outward-dipping setting of inverted L shape liquid collecting plate 59, liquid cylinder 58 is fixed on liquid trap ring 56, the periphery of liquid trap ring 56 is fixed on the inwall of hypomere cylindrical shell 3, liquid trap ring 56, intercepting basin 57 is formed between liquid cylinder 58 and hypomere cylindrical shell 3 three, liquid cylinder 58 is communicated with distribution piping 54 respectively by downtake 55 with intercepting basin 57, the lower surface of distribution piping 54 is evenly equipped with several distribution showerhead 53, the below of distribution showerhead 53 is provided with one-level distribution trough 52, the lower surface of one-level distribution trough 52 is evenly equipped with several secondary distribution grooves 51.
Above-mentioned explanation is not limitation of the utility model, and the utility model is also not limited to above-mentioned citing.Those skilled in the art are in essential scope of the present utility model, and the change made, remodeling, interpolation or replacement, also should belong to protection domain of the present utility model, and protection domain of the present utility model is as the criterion with claims.

Claims (3)

1. the equipment of a preparing silane with trichlorosilane, it is characterized in that: comprise the hypomere cylindrical shell that diameter from bottom to top successively decreases successively, stage casing cylindrical shell, epimere cylindrical shell, described hypomere cylindrical shell is connected by lower conical shell one with described stage casing cylindrical shell, described stage casing cylindrical shell is connected by upper conical shell one with described epimere cylindrical shell, described hypomere cylindrical shell and described stage casing cylindrical shell are separated by spherical lower cover and described lower cover is positioned at the below of described lower conical shell, described stage casing cylindrical shell and described epimere cylindrical shell are separated by spherical upper cover and described upper cover is positioned at the below of described upper conical shell, the bottom of described hypomere cylindrical shell is provided with bottom bulkhead, the top of described epimere cylindrical shell is provided with top end socket,
The barrel top of described hypomere cylindrical shell is provided with hypomere overhead-liquid entrance and the outlet of hypomere top gas, extend the center in described hypomere cylindrical shell in described hypomere overhead-liquid entrance and connect the charging distribution pipe being positioned at described hypomere cylindrical shell, the below of the described charging distribution pipe described in hypomere cylindrical shell inherence is provided with a hypomere catalyst layer, two-layer hypomere packing layer is provided with below the described lower section catalyst layer described in hypomere cylindrical shell inherence, hypomere liquid distributor is provided with between described charging distribution pipe and described lower section catalyst layer, liquid collecting redistributor is respectively arranged with between hypomere packing layer between described lower section catalyst layer and the hypomere packing layer described in upper strata and described in upper strata and the hypomere packing layer described in lower floor, described bottom bulkhead is provided with hypomere bottom liquid outlet,
The barrel top of described stage casing cylindrical shell is provided with stage casing overhead-liquid entrance and the outlet of stage casing top gas, the center in described stage casing cylindrical shell is extended in described stage casing overhead-liquid entrance, stage casing liquid distributor is provided with below the described stage casing overhead-liquid entrance described in cylindrical shell inherence, stage casing, stage casing catalyst layer is provided with below the described stage casing liquid distributor described in cylindrical shell inherence, stage casing, described lower conical shell is provided with stage casing bottom gas inlet, and the bottom of described lower conical shell is provided with stage casing bottom liquid outlet;
The barrel top of described epimere cylindrical shell is provided with epimere overhead-liquid entrance, the center in described epimere cylindrical shell is extended in described epimere overhead-liquid entrance, the described epimere overhead-liquid entrance top described in epimere cylindrical shell inherence is provided with scum dredger, epimere liquid distributor is provided with below the described epimere overhead-liquid entrance described in epimere cylindrical shell inherence, epimere packing layer is provided with below the described epimere liquid distributor described in epimere cylindrical shell inherence, described upper conical shell is provided with epimere bottom gas inlet, the bottom of described upper conical shell is provided with epimere bottom liquid outlet, described top end socket is provided with the outlet of epimere top gas.
2. the equipment of a kind of preparing silane with trichlorosilane according to claim 1, it is characterized in that: described liquid collecting redistributor comprises several inverted L shape liquid collecting plates, liquid cylinder, liquid trap ring, downtake, distribution piping, distribution showerhead, one-level distribution trough and secondary distribution groove, described inverted L shape liquid collecting plate is positioned at the top of described liquid cylinder, described inverted L shape liquid collecting plate is symmetrically distributed in the both sides of described liquid cylinder and the described outward-dipping setting of inverted L shape liquid collecting plate, described liquid cylinder is fixed on described liquid trap ring, the periphery of described liquid trap ring is fixed on the inwall of described hypomere cylindrical shell, described liquid trap ring, intercepting basin is formed between described liquid cylinder and described hypomere cylindrical shell three, described liquid cylinder is communicated with described distribution piping respectively by described downtake with described intercepting basin, the lower surface of described distribution piping is evenly equipped with several distribution showerhead, the below of described distribution showerhead is provided with one-level distribution trough, the lower surface of described one-level distribution trough is evenly equipped with several secondary distribution grooves.
3. the equipment of a kind of preparing silane with trichlorosilane according to claim 2, it is characterized in that: the diameter of described hypomere cylindrical shell is 1 ~ 3 meter, the diameter of described stage casing cylindrical shell is 0.6 ~ 1.5 meter, the diameter of described epimere cylindrical shell is 0.3 ~ 1 meter, the height of described lower section catalyst layer is 1 ~ 4 meter, the height of described hypomere packing layer is 1 ~ 4 meter, and the height of described stage casing catalyst layer is 1 ~ 4 meter, and the height of described epimere packing layer is 1 ~ 4 meter.
CN201520320211.3U 2015-05-18 2015-05-18 A kind of equipment of preparing silane with trichlorosilane Active CN204643856U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925813A (en) * 2015-05-18 2015-09-23 中国化学赛鼎宁波工程有限公司 Trichlorosilan device for preparing silane and method therefor
CN106006647A (en) * 2016-05-17 2016-10-12 山东瑞川硅业有限公司 Trichlorosilane synthesis furnace

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925813A (en) * 2015-05-18 2015-09-23 中国化学赛鼎宁波工程有限公司 Trichlorosilan device for preparing silane and method therefor
CN106006647A (en) * 2016-05-17 2016-10-12 山东瑞川硅业有限公司 Trichlorosilane synthesis furnace
CN106006647B (en) * 2016-05-17 2018-03-13 山东瑞川硅业有限公司 Trichlorosilane synthetic furnace

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Effective date of registration: 20190128

Address after: 461000 Xiangcheng Coal Coking Circular Economy Industrial Park, Xuchang City, Henan Province

Patentee after: Henan silane science and technology development Limited by Share Ltd

Address before: 315040 Lane No. 999, Yangfan Road, R&D Park, Ningbo National High-tech Zone, Zhejiang Province

Patentee before: Sedin Ningbo Engineering Co., Ltd.