CN110697723A - A kind of method utilizing chlorosilane raffinate to prepare silicon dioxide and phosphoric acid and its sodium salt - Google Patents
A kind of method utilizing chlorosilane raffinate to prepare silicon dioxide and phosphoric acid and its sodium salt Download PDFInfo
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Abstract
本发明公开了一种利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括：将氯硅烷残液和磷酸钠盐饱和溶液混合，并通过改变磷酸钠盐饱和溶液的加量调节混合后得到的二氧化硅前驱物悬浊液的pH值；将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为6‑8，然后将滤饼干燥，制得二氧化硅，将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。本发明避免了盐酸溶液的大量挥发对环境的污染、设备的腐蚀及人员的伤害，降低设备成本，维护了生产人员健康。本发明可以根据需要调整生产工艺，获得二氧化硅和磷酸及其盐或者二氧化硅和盐酸溶液，得到产品多样，应用范围广。The invention discloses a method for preparing silicon dioxide, phosphoric acid and its sodium salt by using chlorosilane residual liquid, comprising: mixing the residual chlorosilane liquid and a saturated sodium phosphate solution, and changing the amount of the saturated sodium phosphate solution by changing the dosage Adjusting the pH value of the silica precursor suspension obtained after mixing; filtering the silica precursor suspension, washing the obtained filter cake to a pH value of 6-8, and then drying the filter cake to obtain Silicon dioxide, the obtained filtrate is concentrated and crystallized, the crystal and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid. The invention avoids environmental pollution, equipment corrosion and personnel injury caused by a large amount of volatilization of the hydrochloric acid solution, reduces equipment cost, and maintains the health of production personnel. According to the present invention, the production process can be adjusted as required, and silicon dioxide and phosphoric acid and its salts or silicon dioxide and hydrochloric acid solutions can be obtained, and various products can be obtained, and the application range is wide.
Description
技术领域technical field
本发明涉及氯硅烷残液回收利用以及二氧化硅、磷酸及其钠盐的制备技术领域，具体涉及一种利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法。The invention relates to the technical field of recycling and utilization of chlorosilane residual liquid and the preparation of silicon dioxide, phosphoric acid and their sodium salts, in particular to a method for preparing silicon dioxide, phosphoric acid and their sodium salts by using chlorosilane residual liquid.
背景技术Background technique
氯硅烷残液水解产生盐酸溶液和无定型二氧化硅。盐酸溶液具有很强的挥发性，生产环境恶劣，对设备腐蚀严重，同时对人身健康产生损害。且制备的盐酸溶液的浓度较低，浓缩回收耗能高。因此，通常的方法是将盐酸溶液通入碳酸钙悬浊液中，将盐酸溶液转化为不挥发的氯化钙。然而氯化钙在工业上用量不高，长期堆砌，占用大量场地，对盐酸资源亦是浪费，没有真正利用氯硅烷残液。Hydrolysis of the chlorosilane raffinate yields hydrochloric acid solution and amorphous silica. Hydrochloric acid solution has strong volatility, harsh production environment, serious corrosion to equipment, and damage to human health at the same time. Moreover, the concentration of the prepared hydrochloric acid solution is low, and the energy consumption for concentration and recovery is high. Therefore, the usual method is to pass the hydrochloric acid solution into the calcium carbonate suspension to convert the hydrochloric acid solution into non-volatile calcium chloride. However, the industrial dosage of calcium chloride is not high, and it is piled up for a long time, occupying a lot of space, and it is also a waste of hydrochloric acid resources, and the chlorosilane residue is not really used.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，以解决现有氯硅烷残液利用率低的问题。The object of the present invention is to provide a method for preparing silicon dioxide, phosphoric acid and its sodium salt from chlorosilane raffinate, so as to solve the problem of low utilization rate of existing chlorosilane raffinate.
本发明解决上述技术问题的技术方案如下：The technical scheme that the present invention solves the above-mentioned technical problems is as follows:
一种利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括：将氯硅烷残液和磷酸钠盐饱和溶液混合，得到二氧化硅前驱物悬浊液，并通过改变磷酸钠盐饱和溶液的加量调节二氧化硅前驱物悬浊液的pH值；将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为6-8，然后将滤饼干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸盐、氯化钠，得到的溶液为磷酸。A method for preparing silicon dioxide and phosphoric acid and its sodium salt by using chlorosilane residual liquid, comprising: mixing the residual chlorosilane liquid and a saturated solution of sodium phosphate salt to obtain a silica precursor suspension, and changing the sodium phosphate by changing The addition of the saturated salt solution adjusts the pH value of the silica precursor suspension; the silica precursor suspension is filtered, the obtained filter cake is washed with water to a pH value of 6-8, and then the filter cake is dried, Silica is obtained. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated. The obtained crystals are phosphate and sodium chloride, and the obtained solution is phosphoric acid.
本发明通过将氯硅烷残液通入磷酸钠饱和溶液，使得氯硅烷残液中主要成分如四氯化硅等与水反应产生二氧化硅前驱物沉淀和盐酸溶液，盐酸会使得加入的低品位磷酸钠盐转化为高品位的磷酸钠盐或磷酸。将沉淀过滤，并高温干燥制得无定型二氧化硅粉体。滤液中的氯化氢与外加的磷酸钠盐饱和溶液中的磷酸钠盐反应，控制溶液的pH值和磷酸钠的加入量，使得加入的磷酸钠盐转化为磷酸二氢钠、磷酸氢钠或者磷酸，同时生成氯化钠。In the present invention, the chlorosilane residual liquid is passed into the saturated sodium phosphate solution, so that the main components in the chlorosilane residual liquid, such as silicon tetrachloride, etc., react with water to produce silica precursor precipitation and hydrochloric acid solution, and the hydrochloric acid will make the added low-grade Sodium phosphate is converted into high-grade sodium phosphate or phosphoric acid. The precipitate was filtered and dried at high temperature to obtain amorphous silica powder. The hydrogen chloride in the filtrate reacts with the sodium phosphate in the added sodium phosphate saturated solution, and the pH value of the solution and the amount of sodium phosphate added are controlled, so that the added sodium phosphate is converted into sodium dihydrogen phosphate, sodium hydrogen phosphate or phosphoric acid, At the same time, sodium chloride is formed.
氯硅烷残液中的主要成分SiCl4与水的主要反应为：The main reaction of the main component SiCl 4 in the chlorosilane residue with water is:
SiCl4+2H2O→SiO2↓+4HCl。SiCl 4 +2H 2 O→SiO 2 ↓+4HCl.
因此，氯硅烷残液水解即可得到二氧化硅和盐酸。Therefore, the chlorosilane residue can be hydrolyzed to obtain silica and hydrochloric acid.
磷酸钠与生成的盐酸的主要反应如下：The main reaction of sodium phosphate with the generated hydrochloric acid is as follows:
Na3PO4+HCl→Na2HPO4+NaCl；Na 3 PO 4 +HCl→Na 2 HPO 4 +NaCl;
Na3PO4+2HCl→NaH2PO4+2NaCl；Na 3 PO 4 +2HCl→NaH 2 PO 4 +2NaCl;
Na3PO4+3HCl→H3PO4+3NaCl；Na 3 PO 4 +3HCl→H 3 PO 4 +3NaCl;
通过改变所述磷酸钠盐饱和溶液的加量，使得溶液中，磷酸钠与不同摩尔比的盐酸就你行反应，使加入的磷酸钠转化为磷酸二氢钠、磷酸氢钠或者磷酸。具体获得那种物质，取决于溶液的pH的控制。通过改变磷酸钠盐饱和溶液的加量调节二氧化硅前驱物悬浊液的pH，当pH＜1,主产物为磷酸；pH≈4.7，主产物为磷酸二氢钠；pH≈10,主产物为磷酸氢二钠。由此，获得不同的磷酸盐和磷酸。By changing the addition amount of the saturated sodium phosphate solution, in the solution, sodium phosphate and hydrochloric acid with different molar ratios can be reacted, so that the added sodium phosphate is converted into sodium dihydrogen phosphate, sodium hydrogen phosphate or phosphoric acid. Which substance is obtained depends on the control of the pH of the solution. Adjust the pH of the silica precursor suspension by changing the amount of sodium phosphate saturated solution. When pH<1, the main product is phosphoric acid; pH≈4.7, the main product is sodium dihydrogen phosphate; pH≈10, the main product For disodium hydrogen phosphate. Thereby, different phosphates and phosphoric acids are obtained.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:(18-22)，得到的二氧化硅前驱物悬浊液的pH为8-8.5。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate and the saturated sodium phosphate solution is 1:(18-22), and the pH of the obtained silica precursor suspension is 8 -8.5.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:20。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate to the saturated sodium phosphate solution is 1:20.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:(8-12)，得到的二氧化硅前驱物悬浊液的pH为4-4.5。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate and the saturated sodium phosphate solution is 1:(8-12), and the pH of the obtained silica precursor suspension is 4 -4.5.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:10。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate to the saturated sodium phosphate solution is 1:10.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:(2-6)，得到的二氧化硅前驱物悬浊液的pH为1-2.5。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate and the saturated sodium phosphate solution is 1:(2-6), and the pH of the obtained silica precursor suspension is 1 -2.5.
进一步地，在本发明较佳的实施例中，上述氯硅烷残液和磷酸钠盐饱和溶液的质量比为1:5或1:3。Further, in a preferred embodiment of the present invention, the mass ratio of the above-mentioned chlorosilane raffinate to the saturated sodium phosphate solution is 1:5 or 1:3.
进一步地，在本发明较佳的实施例中，上述磷酸钠盐饱和溶液为磷酸三钠饱和溶液。Further, in a preferred embodiment of the present invention, the above-mentioned saturated sodium phosphate solution is a saturated solution of trisodium phosphate.
进一步地，在本发明较佳的实施例中，上述滤饼的干燥温度为120-180℃。Further, in a preferred embodiment of the present invention, the drying temperature of the filter cake is 120-180°C.
进一步地，在本发明较佳的实施例中，得到的晶体为磷酸氢二钠、磷酸二氢钠或氯化钠。Further, in a preferred embodiment of the present invention, the obtained crystals are disodium hydrogen phosphate, sodium dihydrogen phosphate or sodium chloride.
本发明具有以下有益效果：The present invention has the following beneficial effects:
本发明将氯硅烷残液水解产生的盐酸转化为磷酸及其盐溶液，避免了盐酸溶液的大量挥发对环境的污染、设备的腐蚀及人员的伤害，降低设备成本，维护了生产人员健康。本发明通过添加低品位磷酸钠盐可以制得高品位磷酸、磷酸氢二钠、磷酸二氢钠、氯化钠。The method converts the hydrochloric acid produced by the hydrolysis of the chlorosilane residual liquid into phosphoric acid and its salt solution, avoids environmental pollution, equipment corrosion and personnel injury caused by a large amount of volatilization of the hydrochloric acid solution, reduces equipment costs, and maintains the health of production personnel. In the present invention, high-grade phosphoric acid, disodium hydrogen phosphate, sodium dihydrogen phosphate and sodium chloride can be prepared by adding low-grade phosphate sodium salt.
本发明通过磷酸钠盐饱和溶液来控制溶液的pH值变化范围，进而控制氯硅烷残液的水解速度，利于获得质量稳定的不定型二氧化硅粉体。通过调整氯硅烷残液加入速度，可得到不同比表面积的不定型二氧化硅。1L/h至3L/h的加入速度，获得的二氧化硅的比表面积可在100m2/g至500m2/g之间。不同比表面大小的二氧化硅在作为催化剂载体的负载能力会有很大不同。作为分散剂在溶液中能形成均一溶液，便于溶液的稳定放置。In the present invention, the pH value variation range of the solution is controlled by the saturated sodium phosphate solution, and the hydrolysis speed of the chlorosilane residue is further controlled, which is beneficial to obtain amorphous silica powder with stable quality. Unshaped silica with different specific surface area can be obtained by adjusting the adding speed of chlorosilane residual liquid. With the addition rate of 1 L/h to 3 L/h, the specific surface area of the obtained silica can be between 100 m 2 /g and 500 m 2 /g. Silicas with different specific surface sizes have very different loading capacities as catalyst supports. As a dispersant, it can form a homogeneous solution in the solution, which is convenient for the stable placement of the solution.
本发明可以根据需要调整生产工艺，获得二氧化硅和磷酸及其盐或者二氧化硅和盐酸溶液，得到产品多样，应用范围广。According to the present invention, the production process can be adjusted as required, and silicon dioxide and phosphoric acid and its salts or silicon dioxide and hydrochloric acid solutions can be obtained, and various products can be obtained, and the application range is wide.
具体实施方式Detailed ways
以下结合实施例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。The principles and features of the present invention will be described below with reference to the embodiments. The examples are only used to explain the present invention, but not to limit the scope of the present invention. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased from the market.
实施例1：Example 1:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和磷酸三钠饱和溶液混合按照1:18的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为8。The chlorosilane residual liquid and the trisodium phosphate saturated solution were mixed according to the mass ratio of 1:18, and the pH value of the obtained silica precursor suspension was 8.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为6，然后将滤饼在120℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water to a pH value of 6, and then the filter cake was dried at 120° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例2：Example 2:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和磷酸三钠饱和溶液混合按照1:22的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为8.5。The chlorosilane residual liquid and the saturated trisodium phosphate solution were mixed according to the mass ratio of 1:22, and the pH value of the obtained silica precursor suspension was 8.5.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为6-8，然后将滤饼在180℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water to a pH value of 6-8, and then the filter cake was dried at 180° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例3：Example 3:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和工业十二水磷酸钠饱和溶液混合按照1:20的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为8.2。The chlorosilane residual liquid and the industrial saturated sodium phosphate dodecahydrate solution were mixed according to the mass ratio of 1:20, and the pH value of the obtained silica precursor suspension was 8.2.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例4：Example 4:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和工业十二水磷酸钠饱和溶液混合按照1：8的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为4。The chlorosilane residual liquid and the industrial saturated sodium phosphate dodecahydrate solution are mixed according to the mass ratio of 1:8, and the pH value of the obtained silica precursor suspension is 4.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为6，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water to a pH value of 6, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例5：Example 5:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和工业十二水磷酸钠饱和溶液混合按照1：12的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为4.5。The chlorosilane residual liquid and the industrial saturated sodium phosphate dodecahydrate solution were mixed according to the mass ratio of 1:12, and the pH value of the obtained silica precursor suspension was 4.5.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为8，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water to a pH value of 8, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例6：Example 6:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和磷酸三钠饱和溶液混合按照1:10的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为4.2。The chlorosilane residual liquid and the saturated trisodium phosphate solution were mixed according to the mass ratio of 1:10, and the pH value of the obtained silica precursor suspension was 4.2.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例7：Example 7:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和磷酸三钠饱和溶液混合按照1:2的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为1。The chlorosilane residual liquid and the trisodium phosphate saturated solution are mixed according to the mass ratio of 1:2, and the pH value of the obtained silica precursor suspension is 1.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例8：Example 8:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和磷酸三钠饱和溶液混合按照1:6的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为2.5。The chlorosilane residual liquid and the saturated trisodium phosphate solution were mixed according to the mass ratio of 1:6, and the pH value of the obtained silica precursor suspension was 2.5.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例9：Example 9:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和工业十二水磷酸钠饱和溶液混合按照1:3的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为1.5。The chlorosilane residual liquid and the industrial saturated sodium phosphate dodecahydrate solution are mixed according to the mass ratio of 1:3, and the pH value of the obtained silica precursor suspension is 1.5.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
实施例10：Example 10:
本实施例的利用氯硅烷残液制备二氧化硅和磷酸及其钠盐的方法，包括以下步骤：The method for preparing silicon dioxide and phosphoric acid and its sodium salt by utilizing chlorosilane raffinate of the present embodiment comprises the following steps:
将氯硅烷残液和工业十二水磷酸钠饱和溶液混合按照1:5的质量比混合，得到的二氧化硅前驱物悬浊液的pH值为2。The chlorosilane residual liquid and the industrial saturated sodium phosphate dodecahydrate solution are mixed according to the mass ratio of 1:5, and the pH value of the obtained silica precursor suspension is 2.
将二氧化硅前驱物悬浊液过滤，将得到的滤饼水洗至pH值为7，然后将滤饼在150℃下干燥，制得二氧化硅。将得到的滤液浓缩结晶，分离晶体和溶液，得到的晶体为磷酸钠盐，得到的溶液为磷酸。The silica precursor suspension was filtered, the obtained filter cake was washed with water until the pH value was 7, and then the filter cake was dried at 150° C. to obtain silica. The obtained filtrate is concentrated and crystallized, and the crystals and the solution are separated, the obtained crystal is sodium phosphate salt, and the obtained solution is phosphoric acid.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within the range.
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