CN116462199B - A method for removing carbon from waste silicone contacts and waste pulp residues - Google Patents
A method for removing carbon from waste silicone contacts and waste pulp residues Download PDFInfo
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- 239000002699 waste material Substances 0.000 title claims abstract description 95
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229920001296 polysiloxane Polymers 0.000 title description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000012298 atmosphere Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract 5
- 238000007873 sieving Methods 0.000 claims abstract 2
- 239000010802 sludge Substances 0.000 claims 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 229910052710 silicon Inorganic materials 0.000 abstract description 12
- 239000010703 silicon Substances 0.000 abstract description 12
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003723 Smelting Methods 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 239000002054 inoculum Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 description 20
- 239000010431 corundum Substances 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 101100012902 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) FIG2 gene Proteins 0.000 description 1
- 101100233916 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) KAR5 gene Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 elemental silicon) Chemical compound 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003895 groundwater pollution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
Description
技术领域Technical Field
本发明属于有机硅废浆渣、废触体资源化利用技术领域，具体涉及一种去除有机硅废触体和废浆渣中碳的方法。The invention belongs to the technical field of resource utilization of waste organosilicon slurry and waste contacts, and in particular relates to a method for removing carbon from waste organosilicon contacts and waste slurry.
背景技术Background Art
目前国内外有机硅单体的生产普遍采用直接法合成甲基氯硅烷，其生产过程中会产生大量的废浆渣和废触体。废浆渣主要由高沸物和未反应的硅粉、铜粉及少量碳组成，固体含量约为25％；废触体主要含硅70～75％左右(以单质硅为主)，含铜5～10％左右，含碳1～10％。At present, the production of organosilicon monomers at home and abroad generally adopts the direct method to synthesize methylchlorosilane, and a large amount of waste slurry and waste contacts will be generated during the production process. The waste slurry is mainly composed of high boiling points and unreacted silicon powder, copper powder and a small amount of carbon, with a solid content of about 25%; the waste contacts mainly contain about 70-75% silicon (mainly elemental silicon), about 5-10% copper, and 1-10% carbon.
很多企业通过氨浸法、还原法或者其他方式将废触体、废渣浆中的铜提取出来。上述方法只提取了其中10～15％的铜，大量有回收价值的硅粉没有得到资源化利用。废触体和废渣浆中含60～70％的硅粉、3.28～15.83％的碳和2～3％的铁、9～10％的氯及少量的其他杂质，氯通过水洗其去除率达90％。企业对上述废渣处理一般是填埋或焚烧，直接填埋或焚烧都会对环境造成较大影响，焚烧会产生大量有毒气体造成二次污染；填埋会占用较大空间，且析出的物质会导致土壤和地下水被污染。中国专利CN114349010A公开了一种提铜后废硅粉除碳的方法，向提铜后废硅粉中添加OP系列乳化剂、表面活性剂、二丁酯和水等清洗液搅拌静置沉淀，下部沉淀水洗、烘干，将碳含量从3～6％降至1％，其操作过程复杂，还会带来一系列废液处理问题。中国专利CN115181998A公开了一种从有机硅废触体中回收高纯度硅粉的方法，通过加硫酸和调整剂氧化酸浸、浸出渣洗涤压滤，再中和得到纯度98％左右的硅粉，该方法工艺流程长，酸浸存在对设备要求高、污染环境等缺陷。Many companies extract copper from waste contacts and waste slag slurry through ammonia leaching, reduction or other methods. The above methods only extract 10-15% of the copper, and a large amount of silicon powder with recycling value is not utilized as a resource. Waste contacts and waste slag slurry contain 60-70% silicon powder, 3.28-15.83% carbon, 2-3% iron, 9-10% chlorine and a small amount of other impurities. The removal rate of chlorine through water washing is 90%. Companies generally landfill or incinerate the above waste slag. Direct landfill or incineration will have a great impact on the environment. Incineration will produce a large amount of toxic gases and cause secondary pollution; landfill will take up a large space, and the precipitated substances will cause soil and groundwater pollution. Chinese patent CN114349010A discloses a method for removing carbon from waste silicon powder after copper extraction, wherein OP series emulsifiers, surfactants, dibutyl esters and water are added to the waste silicon powder after copper extraction, stirred and allowed to settle, and the lower precipitate is washed and dried to reduce the carbon content from 3-6% to 1%. The operation process is complicated and will also bring a series of waste liquid treatment problems. Chinese patent CN115181998A discloses a method for recovering high-purity silicon powder from waste organic silicon contacts, wherein silicon powder with a purity of about 98% is obtained by adding sulfuric acid and an adjusting agent for oxidation acid leaching, washing and filtering the leached residue, and then neutralizing. The process of this method is long, and the acid leaching has the defects of high equipment requirements and environmental pollution.
因此，为了解决上述问题，本文提出一种去除有机硅废触体和废浆渣中碳的方法。Therefore, in order to solve the above problems, this paper proposes a method for removing carbon from waste silicone contacts and waste pulp.
发明内容Summary of the invention
为了解决上述技术问题，本发明设计了一种去除有机硅废触体和废浆渣中碳的方法In order to solve the above technical problems, the present invention designs a method for removing carbon from waste silicone contacts and waste pulp residues.
为了达到上述技术效果，本发明是通过以下技术方案实现的：一种去除有机硅废触体和废浆渣中碳的方法，其特征在于，包括以下步骤：In order to achieve the above technical effects, the present invention is implemented by the following technical scheme: a method for removing carbon from waste silicone contacts and waste pulp residues, characterized in that it comprises the following steps:
Step1：将有机硅废触体和废浆渣真空干燥，并用振动磨研磨后过50～150目筛网；Step 1: vacuum dry the waste silicone contact body and waste pulp residue, grind them with a vibration mill and pass them through a 50-150 mesh screen;
Step2：研磨后的样品放置于氮气和空气的混合气氛中，在300～500℃下进行氧化焙烧1～8h，得到低碳含量的硅粉。Step 2: The ground sample is placed in a mixed atmosphere of nitrogen and air, and oxidatively calcined at 300-500°C for 1-8 hours to obtain silicon powder with a low carbon content.
进一步的，Step1中所述的筛网为100目。Furthermore, the sieve described in Step 1 is 100 mesh.
进一步的，Step2中所述的氧化焙烧温度为500℃，时间为5h。Furthermore, the oxidation roasting temperature described in Step 2 is 500° C. and the time is 5 h.
进一步的，所述的Step2混合气氛中氮气和空气体积比为1:3～1:5。Furthermore, the volume ratio of nitrogen to air in the mixed atmosphere of Step 2 is 1:3 to 1:5.
进一步的，所述的混合气氛中氮气和空气体积比为1:4。Furthermore, the volume ratio of nitrogen to air in the mixed atmosphere is 1:4.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明所述的一种去除有机硅废触体和废浆渣中碳的方法，通过焙烧，使有机硅废触体和废浆渣中的有机碳得到充分挥发去除，为了控制金属硅粉的氧化，选择低温低氧势焙烧以减缓硅的氧化速度，利用足够长的焙烧时间以保证物料中的无机碳与氧气反应生成一氧化碳或二氧化碳气体逸出，在减少硅氧化的同时提高杂质碳的去除率；通过该工艺所得硅粉的碳含量较低，其性能更优，可作为硅冶炼企业的原料、硅系孕育剂，达到废物再利用的目的。The method for removing carbon from waste organosilicon contacts and waste slurry residues described in the present invention fully volatilizes and removes the organic carbon in the waste organosilicon contacts and waste slurry residues through roasting. In order to control the oxidation of metallic silicon powder, low-temperature and low-oxygen potential roasting is selected to slow down the oxidation rate of silicon. A sufficiently long roasting time is used to ensure that the inorganic carbon in the material reacts with oxygen to generate carbon monoxide or carbon dioxide gas to escape, thereby reducing silicon oxidation and increasing the removal rate of impurity carbon. The silicon powder obtained by this process has a lower carbon content and better performance, and can be used as a raw material and silicon-based inoculant for silicon smelting enterprises to achieve the purpose of waste recycling.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.
图1是本发明去除有机硅废触体、废浆渣中碳的方法的流程示意图；FIG1 is a schematic flow diagram of a method for removing carbon from waste organic silicon contacts and waste pulp residues according to the present invention;
图2是本发明有机硅废触体、废浆渣干燥研磨后的红外光谱分析；FIG2 is an infrared spectrum analysis of the waste silicone contacts and waste pulp residue after drying and grinding of the present invention;
图3是本发明实施例焙烧除碳后得到的低碳含量硅粉的红外光谱分析。FIG3 is an infrared spectrum analysis of the low carbon content silicon powder obtained after calcination and carbon removal according to an embodiment of the present invention.
具体实施方式DETAILED DESCRIPTION
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
实施例1Example 1
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度500℃，在氮气和空气体积比为1:4的混合气氛中保温加热3h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 500° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 3 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达98.23％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 98.23%.
实施例2Example 2
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度500℃，在氮气和空气体积比为1:4的混合气氛中保温加热5h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 500° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 5 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达99.55％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 99.55%.
实施例3Example 3
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度500℃，在氮气和空气体积比为1:4的混合气氛中保温加热1h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 500° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 1 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达83.539％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 83.539%.
实施例4Example 4
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度450℃，在氮气和空气体积比为1:3的混合气氛中保温加热2h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 450° C., and heating for 2 h in a mixed atmosphere of nitrogen and air with a volume ratio of 1:3;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达88.50％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 88.50%.
实施例5Example 5
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度450℃，在氮气和空气体积比为1:4的混合气氛中保温加热3h；(2) taking 20 g of the sample of step (1) and placing it in a corundum boat, and placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 450° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 3 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达94.06％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 94.06%.
实施例6Example 6
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度450℃，在氮气和空气体积比为1:4的混合气氛中保温加热6h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 450° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 6 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达98.92％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 98.92%.
实施例7Example 7
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度400℃，在氮气和空气体积比为1:4的混合气氛中保温加热3h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 400° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 3 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达81.80％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 81.80%.
实施例8Example 8
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度400℃，在氮气和空气体积比为1:4的混合气氛中保温加热7h；(2) taking 20 g of the sample of step (1) and placing it in a corundum boat, and placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 400° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 7 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达98.67％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 98.67%.
实施例9Embodiment 9
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度350℃，在氮气和空气体积比为1:5的混合气氛中保温加热8h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 350° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:5 for 8 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达97.53％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 97.53%.
实施例10Example 10
一种去除有机硅废触体和废浆渣中碳的方法，具体步骤如下：A method for removing carbon from waste silicone contacts and waste pulp residues, the specific steps are as follows:
(1)取一定量的有机硅废触体和废浆渣在真空干燥箱内干燥，将干燥后的样品在振动磨内破碎研磨，至物料全通过100目筛；(1) Take a certain amount of waste silicone contacts and waste pulp residue and dry them in a vacuum drying oven, and crush and grind the dried samples in a vibration mill until all the materials pass through a 100-mesh sieve;
(2)取20g步骤(1)的样品放入刚玉舟中，并将刚玉舟放置于卧式电阻炉中，调节焙烧温度300℃，在氮气和空气体积比为1:4的混合气氛中保温加热3h；(2) taking 20 g of the sample prepared in step (1) and placing it in a corundum boat, placing the corundum boat in a horizontal resistance furnace, adjusting the roasting temperature to 300° C., and heating in a mixed atmosphere of nitrogen and air with a volume ratio of 1:4 for 3 h;
(3)待温度自然冷却到室温后，将样品取出来检测碳含量，其中杂质碳的去除率达45.16％。(3) After the temperature naturally cooled to room temperature, the sample was taken out to detect the carbon content, wherein the removal rate of impurity carbon reached 45.16%.
实施例11Embodiment 11
由附图2和附图3可明显看出，图2中2961.69cm-1对应C-H的特征峰，1260.2cm-1处对应Si-(CH3)2特征吸收峰，经低温焙烧除碳后上述特征峰明显消失，说明低温低氧势焙烧可有效去除有机硅废触体、废浆渣中的有机碳和无机碳。It can be clearly seen from Figures 2 and 3 that 2961.69 cm -1 in Figure 2 corresponds to the characteristic peak of CH, and 1260.2 cm -1 corresponds to the characteristic absorption peak of Si-(CH 3 ) 2. After low-temperature calcination and carbon removal, the above characteristic peaks obviously disappear, indicating that low-temperature and low-oxygen potential calcination can effectively remove organic carbon and inorganic carbon in waste silicone contacts and waste pulp residues.
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