CN1041828C - Organosilicon cyclic body prepared by silastic atmospheric cracking - Google Patents
Organosilicon cyclic body prepared by silastic atmospheric cracking Download PDFInfo
- Publication number
- CN1041828C CN1041828C CN 92112510 CN92112510A CN1041828C CN 1041828 C CN1041828 C CN 1041828C CN 92112510 CN92112510 CN 92112510 CN 92112510 A CN92112510 A CN 92112510A CN 1041828 C CN1041828 C CN 1041828C
- Authority
- CN
- China
- Prior art keywords
- silastic
- catalyst
- organosilicon
- pipe
- ring body
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Silicon Polymers (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention relates to a method for manufacturing organosilicon cyclic compounds by silastic atmospheric pressure cracking, which belongs to the chemical comprehensive utilization of waste and old silastic. The present invention uses scrap and waste materials of silastic products and the waste and old silastic as raw materials which are washed, pulverized, and cracked at the atmospheric pressure and at a temperature of 200 DEG C to 500 DEG C under a catalytic condition for safely producing the organosilicon cyclic compounds. The present invention has the prominent advantages of simple technological equipment, low electrothermal unit consumption, high average one-way yield, safe operation and convenient, economic and continuous or discontinuous production.
Description
The present invention relates to the chemical industry comprehensive utilization of waste silicone rubber, is the manufacture method that a kind of atmospheric cracking silicon rubber prepares the organosilicon ring body.
Current, silicon rubber shared proportion in whole world organosilicon product surpasses 50%, the leftover bits of silastic product, the accumulating amount of waste silicone rubber are also more and more, and these waste silicone rubber major parts are dropped or are only pulverized and do filler, are used for laying road or are used for building waterproof layer.Produce hexamethyl cyclotrisiloxane (D as for directly adopting waste silicone rubber industrialization ground cracking to fall consor
3), the organosilicon ring bodies such as siloxanes of octamethylcyclotetrasiloxane and other big ring, do not meet reported in literature so far as yet.
The objective of the invention is directly to adopt waste silicone rubber is raw material, comprises sulfuration or not sulfuration, contains filler or does not contain the various waste silicone rubbers of filler, and atmospheric cracking is produced the organosilicon ring body.
To achieve these goals, it is poly-that the present invention adopts catalysis to fall, and normal pressure splits Jie's technology.Select for use sulfuration or the sulfuration various waste silicone rubbers that contain filler or do not contain filler be raw material, under the temperature condition of catalyst and 150 ℃～500 ℃, atmospheric cracking methylsiloxane circlewise prepares the organosilicon ring body.At first waste silicone rubber is cleaned up and drain, be ground into fritter or sheet (being used) if silicon rubber viscous fluid or gel also can directly be sneaked into pulverizer; To be cut into small pieces again or flaky silicon rubber and the abundant mix of catalyst, and make the surface of silicon rubber be stained with catalyst equably.Catalyst adopts normally used alkali metal hydroxide or its aqueous solution (concentration is 28～35%).The consumption of catalyst is generally 3～8% of silicon rubber weight of material, 0.2～1.2% of its consumption of adding tensio-active agent in the catalyst.Behind silicon rubber and the even mix of catalyst,, under normal pressure, split Jie's methylsiloxane circlewise from the top mouth charging of scission reaction stove.
The scission reaction stove adopts the vertical structure of blank pipe, can be that single tube also can be a multitube, and how much this can deciding according to reaction mass.
Guan Gaowei 1～the 2m of scission reaction stove, the useful volume of blank pipe is at 0.8m
3More than, around the resistance wire heating, whole scission reaction stove is divided into 2～3 heating zones outward, and the temperature of each heating zone is controlled between 150 ℃～500 ℃, and guarantees to increase piecemeal from epimere to hypomere temperature.Industrially, pyrolysis can be divided into 3 heating zones for being made full use of.Epimere is a preheating section, and temperature is controlled at about 150 ℃～200 ℃; The stage casing is preceding conversion zone, and temperature is controlled at about 200～400 ℃; Hypomere is the afterreaction section, and temperature is controlled at about 300～500 ℃.In the middle of the pipe material stirring rod is housed, is used for ash discharge and loosening gas circuit.Be mixed with the material of catalyst equably, from the charging opening of Reaktionsofen, add, the material steam that reaction generates is discharged from the material steam exit of Reaktionsofen downside, the pressure that reacted residual ash leans on gravity to reach when feeding in raw material moves down automatically, discharge from the ash output hole of Reaktionsofen bottom, ash output hole immerses in the water, and ashes directly enters in the water.
From scission reaction furnace bottom side, the reactant that material vapor outlet port place discharges after the condensation, can obtain organosilicon hybrid ring body through dedusting.
This mixed methylcyclosiloxane contains moisture, uses water-and-oil separator, and water layer is discharged from the bottom, and oil reservoir is discharged by the top, and this oil reservoir is the organosilicon ring body.After measured, it includes the hexamethyl cyclotrisiloxane (D more than 30%
3), the octamethylcyclotetrasiloxane more than 40%, D
3～D
7Being hexamethyl cyclotrisiloxane--the total content of tetradecamethylcycloheptasiloxane reaches more than 90% this organosilicon hybrid ring body and can be directly used in through purified powder system and produce various high-quality organosilicon products.Residual ash after the scission reaction and fail the material piece of complete reaction because of its surface is mixed with the organosilicon thing equably, can directly be recycled.
Adopt the method for atmospheric cracking to produce organosilicon hybrid ring body, operational safety, efficient height, the electric heating unit consumption is low, processing unit simple, can make things convenient for, economically suitability for industrialized production.
Fig. 1 makes the schema of organosilicon hybrid ring body for silicon rubber cracking.
Fig. 2 is a scission reaction stove sectional view.
The reaction process flow process is schematically as follows: the raw material catalyst ↓ ↓ washing → pulverizing → batching → reaction → dedusting → condensation → separation → organosilicon hybrid ring body
As shown in Figure 1, material (1) is put into washing bath (2) washing, through pulverizer (3) fragmentation, sneaks into alkali metal hydroxide or its aqueous solution in material, and tensio-active agent.Evenly mix and stir in agitator (4), put into scission reaction stove (5) by the material mouth then, the material steam that reaction generates is discharged from the material steam exit of Reaktionsofen.Through fly-ash separator (6) and condenser (7), discharge and obtain organosilicon hybrid ring body.
The present invention is illustrated with embodiment below in conjunction with accompanying drawing.
Example one: the example of single tube reactor.
As accompanying drawing 2, the scission reaction stove is a single tube reactor.Adopt directly through Φ 4 ", the steel pipe of long 1000mm.Useful volume 8 liters of blank pipe (9).The outside nichrome wire that twines divides three sections (10), (11), (12) to control three sections Heating temperatures respectively by voltate regulator.Epimere (10) is controlled at about 150 ℃, and stage casing (11) are controlled at 200～400 ℃, hypomere (12) and are controlled at 300～500 ℃; Reactor downside material steam exit (13) is connected to fly-ash separator and prolong.Ash output hole (14) immerses in the water.5kg thickness be the sheet waste silicone rubber of 5mm after washing drains, be cut into the random small pieces of 2～3mm.Sneak into the tensio-active agent that weight is about 6% potassium hydroxide aqueous solution (concentration is 30%) of silicon rubber weight and is about 3g in material, the three evenly mixes and stirs in agitator.Then adopt the interruption method or uninterruptedly add charging opening (7) charging of the method for material from the scission reaction stove, heating is reacted gradually.With loosening material gas circuit of material stirring rod (8) and ash discharge.Initial reaction is more violent, then tends to be steady.Have white cigarette to discharge at material vapor outlet port place (13), through dedusting, condensation, usefulness oil--water separator separation, the upper strata is an organosilicon hybrid ring body, and lower floor is a water.Obtain the thick oily 2.4kg of organosilicon hybrid ring body, recovery per pass reaches 48%.
Example two: the example of two-tube reactor
Prepare a two-tube reactor, its useful volume 200 liters.Reactor head is provided with charging opening, and with the material stirring rod.The reactor bottom reducing is immersed in the water, and ashes directly enters in the water.Raw material select for use mix liquid state is arranged, the organosilicon superpolymer of gel state, adhesion attitude, and the waste silicone rubber that is mingled with the residual ash of part scission reaction.Press the working method of example one, adopt the interruption method or add the uninterrupted dual mode of material midway and produce atmospheric cracking silicon rubber and other organosilicon superpolymer as a trial.Its result such as table one.
Table a pair of pipe reactor The pilot plant result
| Numbering | (kg) feeds intake | Product | Once through yield (%) | Electric heating unit consumption kw/kg (oil) | Remarks | ||
| Silicon rubber | Other sand part | Catalyst | |||||
| 1 | 50 | 25 | 6％ | 40 | 53 | 2．5 | The |
| 2 | 150 | 50 | 6％ | 96 | 48 | 2．4 | Add the material method |
Example three: multitubular reactor suitability for industrialized production
Reactor is zoomed into industrial scale again.Make a multitubular reactor, its useful volume reaches 1000 liters.Reactor head is provided with charging opening, is provided with the material stirring rod in material bed.The partition zone of heating is divided into three heating zones, and is controlled on 150～500 ℃ of each different temperature of reaction sections.Whole reactor and washing, pulverizing, dedusting, condensation, equipment such as separate and form a whole set of complete flow process.As example one operation.Divide first, second, third class Three, the mode of taking every interval to add a defective material in 1～2 hour is produced.Its result such as table two.
The daily output statistics in table two multitubular reactor continuous production three one months of the middle of the month of test manufacture
| Teams and groups' title | Silicon rubber (kg) | Product (oil) kg | Once through yield (%) | Average electrical thermal power (kw) | Average electric heating unit consumption kw/kg (oil) |
| First class | 248 | 124 | 50．2 | 16．4 | 1．06 |
| Second class | 220 | 120 | 54．5 | 15．4 | 1．03 |
| Third class | 229 | 129 | 56．3 | 14．3 | 0．89 |
| Average daily production | 697 | 373 | 53．5 | 15．4 | 0．99 |
Can predict that overcome the leakage of equipment and shortening, the stable pitch time of adding material, once through yield can reach more than 60%.The material steam that atmospheric cracking forms becomes the thick mixed methylcyclosiloxane of organosilicon through dedusting, condensation separation.Through purifying, making with extra care, quality can reach the quality standard with the direct synthetic organosilicon of silica flour siloxanes to this organosilicon hybrid ring body again.Can be directly used in and make various high-quality organosilicon products.
Processing unit of the present invention is simple, operational safety, yield height, electric heating unit consumption are low.Can make things convenient for, suitability for industrialized production economically.Be the comprehensive utilization of waste silicone rubber, suitability for industrialized production organosilicon ring body has been opened up a new field.
Claims (2)
1. manufacture method for preparing the organosilicon ring body with silicon rubber, it is characterized in that: selecting waste silicone rubber for use is raw material, comprise sulfuration or not sulfuration, contain filler or do not contain the waste silicone rubber of filler, drain through washing, pulverize and all mix in the scission reaction stove of packing into catalyst, atmospheric cracking methylsiloxane ring body circlewise under 150 ℃～500 ℃ reaction conditions, used catalyst is alkali metal hydroxide or its aqueous solution in the reaction, concentration is 28～35%, the consumption of catalyst is 3～8% of a raw material weight, and being added with tensio-active agent, its consumption is 0.2～1.2% of a catalyst.
2. scission reaction stove according to claim 1 adopts the blank pipe vertical structure, and the pipe number of reactor can be single tube or multitube, and the height of pipe is 1～2m, and useful volume is at 0.8m
3More than, the material stirring rod is housed in the pipe, adopt the tube exterior subsection heating, can be 2～3 heating zones, the temperature of each heating zone raises from top to bottom piecemeal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112510 CN1041828C (en) | 1992-11-05 | 1992-11-05 | Organosilicon cyclic body prepared by silastic atmospheric cracking |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112510 CN1041828C (en) | 1992-11-05 | 1992-11-05 | Organosilicon cyclic body prepared by silastic atmospheric cracking |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1086518A CN1086518A (en) | 1994-05-11 |
| CN1041828C true CN1041828C (en) | 1999-01-27 |
Family
ID=4945977
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92112510 Expired - Fee Related CN1041828C (en) | 1992-11-05 | 1992-11-05 | Organosilicon cyclic body prepared by silastic atmospheric cracking |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041828C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6262289B1 (en) | 1997-06-11 | 2001-07-17 | Kaneka Corporation | Process for preparing cyclic oligosiloxanes |
| CN1111560C (en) * | 1999-11-09 | 2003-06-18 | 陈彦霖 | A kind of method that from the silicon rubber waste product, reclaims silicon monomer |
| CN103626796A (en) * | 2012-08-28 | 2014-03-12 | 杨晓林 | Recovery method of silicone rubber |
-
1992
- 1992-11-05 CN CN 92112510 patent/CN1041828C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1086518A (en) | 1994-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102030329B (en) | Polycrystalline silicon producing device and process | |
| CN106635115B (en) | Utilize the method and hydro-thermal reaction system of mixed waste plastic rubbish high-efficiency cleaning liquefaction | |
| CN1027809C (en) | Method for synthesizing paraffin chloride | |
| CN1041828C (en) | Organosilicon cyclic body prepared by silastic atmospheric cracking | |
| CN105174262B (en) | The apparatus and method of heat accumulating type calcium carbide production technology coproduction by acetic acid ethene | |
| CN1259391C (en) | Method of cracking heavy hydrocarbon to prepare low-carbon olefin and the cracking gasifier system | |
| CN103570760B (en) | Hydroxy ethylene diphosphonic acid production unit and method thereof | |
| CN206266493U (en) | The system that a kind of coal is classified dual treatment | |
| CN106281398A (en) | A kind of coal heat decomposition stove and pyrolysis of coal method | |
| CN106479547A (en) | The system and method that a kind of coal is classified dual treatment | |
| CN108484658A (en) | Hexamethyldisiloxane production method | |
| CN104556054B (en) | The recoverying and utilizing method and device of light component in trichlorosilane synthesis material | |
| CN1102605C (en) | Process for treating waste rubber or plastics and its gasifying equipment | |
| CN105062568B (en) | Method for utilizing coal and natural gas jointly to produce synthesis gas | |
| CN101579611A (en) | Device for preparing methyl chloride and ammonia and method thereof | |
| CN205710607U (en) | A kind of device utilizing coke to prepare LNG unstripped gas | |
| CN106497606B (en) | Coal direct hydrogenation method for pyrolysis | |
| CN210826069U (en) | Upper and lower double-heat high-resolution suspension bed reaction device | |
| CN110835554B (en) | Method for catalyzing steam gasification of bituminous coal by carbide slag | |
| CN110423887B (en) | Device and process for continuously treating waste metal sodium by utilizing potassium hydroxide | |
| CN111747849A (en) | Method for synthesizing n-propyl acetate by continuous catalytic esterification of benzenesulfonic acid and derivatives thereof | |
| CN208829608U (en) | Phyteral converts the efficient multi-product unit of new energy | |
| CN217910365U (en) | Coke inhibitor production equipment system for inhibiting coking of light hydrocarbon cracking furnace tube | |
| CN208151289U (en) | A kind of novel plastic oil refining furnace | |
| CN219972210U (en) | System for cooperatively disposing biochemical sludge by utilizing multi-nozzle opposite gasification furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C53 | Correction of patent for invention or patent application | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: CHEN ZHENGQI; WENG SUHUA TO: CHEN ZHENGQI |
|
| CP03 | Change of name, title or address |
Address after: 228 361004, four, 401, Hubin South Road, Fujian, Xiamen Inventor after: Chen Zhengqi Patentee after: Chen Zhengqi Address before: 100073, 19 West Third Ring Road, 93, 5, two, gate, No. Beijing Inventor before: Chen Zhengqi Patentee before: Weng Suhua Inventor before: Weng Suhua Patentee before: Chen Zhengqi |
|
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |