阅读说明：本技术 一种硫磺悬浮分离剂及其制备方法和应用 (Sulfur suspension separating agent and preparation method and application thereof ) 是由 易玉峰 陈晗旭 黄龙 丁福臣 李艳静 李卫华 李新 于 2019-10-08 设计创作，主要内容包括：本发明公开了一种硫磺悬浮分离剂及其制备方法和应用。本发明中的硫磺悬浮分离剂按照重量份数计,包括非离子型表面活性剂5～10份、非离子型乳化剂2～4份、二氧化硅0.5～2份、增稠剂0.5～2份。本发明的硫磺悬浮分离剂可以直接应用在吸附剂的空气氧化过程中,无需吸附剂达到使用寿命后再取出进行硫磺与羟基氧化铁之间的分离操作,操作十分简便。(The invention discloses a sulfur suspension separating agent, a preparation method and application thereof. The sulfur suspension separating agent comprises, by weight, 5-10 parts of a nonionic surfactant, 2-4 parts of a nonionic emulsifier, 0.5-2 parts of silicon dioxide and 0.5-2 parts of a thickening agent. The sulfur suspension separating agent can be directly applied to the air oxidation process of the adsorbent, the adsorbent does not need to be taken out after reaching the service life to carry out the separation operation between the sulfur and the iron oxyhydroxide, and the operation is very simple and convenient.)

1. The sulfur suspension separating agent is characterized by comprising the following raw materials in parts by weight:

5-10 parts of a nonionic surfactant;

2-4 parts of a non-ionic emulsifier;

0.5-2 parts of silicon dioxide;

0.5-2 parts of a thickening agent.

2. The sulfur suspension separation agent according to claim 1, wherein the nonionic surfactant is at least two of perfluoro silicone oil, methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl trifluoropropyl silicone oil and fluoroether modified silicone oil.

3. A sulphur suspension separator according to claim 1 or 2, wherein the non-ionic emulsifier is at least two of span 60, span 80, tween 60 and tween 80.

4. A sulphur suspension separator according to any of claims 1 to 3, wherein the silica is nanoscaled silica.

5. A sulphur suspension separation agent according to any of claims 1 to 4, wherein the thickener is one or more of guar gum, sesbania gum and derivatives thereof, sodium carboxymethylcellulose.

6. A sulphur suspension separator according to any of claims 1 to 5, further comprising 83 to 92 parts of deionized water.

7. A preparation process of a sulfur suspension separating agent is characterized by comprising the following steps:

uniformly mixing a thickening agent with water to obtain a thickening agent aqueous solution, and uniformly mixing a non-ionic emulsifier with water to obtain an emulsifier solution;

slowly adding a nonionic surfactant and silicon dioxide into the emulsifier solution under the stirring condition of 35-55 ℃, heating, accelerating stirring and uniformly mixing to prepare a uniform mixed solution, adding a thickening agent aqueous solution, continuously stirring and mixing, and cooling to room temperature to obtain a finished product.

8. The preparation process of the sulfur suspension separation agent according to claim 7, wherein the temperature during the heating and accelerated stirring and mixing is 60-80 ℃, and the time for continuously stirring and mixing is 1-3 h.

9. Use of a sulphur suspension separator according to any of claims 1 to 6 or a sulphur suspension separator prepared by the process according to claim 7 or 8.

10. The use according to claim 9, wherein the sulphur suspension separation agent is used in a desulfurization sorbent regeneration process.

11. Use according to claim 9, wherein the sulphur suspension separation agent is added to the regeneration tank of the slurry bed to effect sulphur separation.

Technical Field

The invention relates to the field of sulfur separation, and in particular relates to a sulfur suspension separating agent, and a preparation method and application thereof.

Background

The slurry bed process is one of the industrially used techniques for removing hydrogen sulfide. The slurry bed method adopts iron oxyhydroxide slurry as an adsorbent to absorb hydrogen sulfide in an absorption reactor, and the generated iron sulfydryl sulfide is oxidized and regenerated by air in a regeneration tank to generate iron oxyhydroxide which is then returned to the absorption reactor for recycling. The technology has good operation flexibility and low operation cost. However, sulfur generated by reduction in the operation process is easily attached to the adsorbent generated by air oxidation regeneration, so that the adsorption active center of the adsorbent is covered, the adsorption efficiency of the adsorbent is reduced, and the adsorbent is gradually disabled.

Disclosure of Invention

The technical problem to be solved by the invention is that the adsorbent in the prior art is basically disassembled for desulfurization treatment after the adsorbent reaches the service life, and the separation treatment method for desulfurization is relatively complicated; provides a sulfur suspension separation agent which can simply remove sulfur adsorbed on an adsorbent in a life period, and discloses an application of the sulfur suspension separation agent.

A sulfur suspension separating agent comprises the following raw materials in parts by weight:

5-10 parts of a nonionic surfactant;

2-4 parts of a non-ionic emulsifier;

0.5-2 parts of silicon dioxide;

0.5-2 parts of a thickening agent.

The nonionic surfactant is at least two of perfluoro silicone oil, methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl trifluoro propyl silicone oil and fluorine ether modified silicone oil.

The non-ionic emulsifier is at least two of span 60, span 80, Tween 60 and Tween 80.

The silicon dioxide is nano-scale silicon dioxide.

The thickening agent is one or more of guar gum, sesbania gum and derivatives thereof, and sodium carboxymethyl cellulose.

The sulfur suspension separating agent provided by the invention further comprises 83-92 parts of deionized water as raw materials.

A preparation process of a sulfur suspension separating agent comprises the following steps:

uniformly mixing a thickening agent with water to obtain a thickening agent aqueous solution, and uniformly mixing a non-ionic emulsifier with water to obtain an emulsifier solution;

slowly adding a nonionic surfactant and silicon dioxide into the emulsifier solution under the stirring condition of 35-55 ℃, heating, accelerating stirring and uniformly mixing to prepare a uniform mixed solution, adding a thickening agent aqueous solution, continuously stirring and mixing, and cooling to room temperature to obtain a finished product.

The temperature when the mixture is uniformly stirred and mixed is increased by accelerating the temperature rise is 60-80 ℃, and the time for continuously stirring and mixing is 1-3 h.

The invention also discloses an application of the sulfur suspension separating agent. In particular to the application of the sulfur suspension separating agent in the regeneration process of a desulfurization adsorbent.

More specifically, the sulfur suspension separating agent is added into a regeneration groove of a slurry bed to realize the separation of sulfur.

The liquid in the lower part of the regeneration tank is returned to the absorption reactor of the slurry bed by a pump.

The technical scheme of the invention has the following advantages:

1. because the hydroxyl ferric sulfide is prone to hydrophilicity, the powder contact angle of the hydroxyl ferric sulfide is 20-30 degrees, the sulfur is prone to hydrophobicity, and the powder contact angle of the sulfur is 80-90 degrees, the invention utilizes the difference between the hydrophilicity and the hydrophobicity between the sulfur and the hydroxyl ferric sulfide, adds the sulfur suspension separating agent for adjusting the wettability, the sulfur suspension separating agent comprises 5-10 parts of nonionic surfactant, 2-4 parts of nonionic emulsifier, 0.5-2 parts of silicon dioxide and 0.5-2 parts of thickening agent, through the compounding of the components, the sulfur can be suspended and separated and enriched to the upper part of the liquid surface to form a sulfur froth layer with certain structural strength, the adsorbent is settled at the middle lower part of the liquid, the purpose of separating the adsorbent from the sulfur is achieved, only the sulfur froth layer needs to be floated during the separation, and the sulfur suspension separating agent can be directly applied to the air oxidation process of the adsorbent, the adsorbent is not required to be taken out after reaching the service life for carrying out the separation operation between the sulfur and the iron oxyhydroxide, and the operation is very simple and convenient. Meanwhile, after hydrophilic fine-particle-size powdery iron hydroxysulfide is adsorbed or subjected to in-situ reaction to generate fine-particle hydrophobic sulfur, the hydrophilic and hydrophobic groups are provided, so that the hydrophilic and hydrophobic groups play a role similar to a surfactant and easily cause a foaming problem; according to the invention, through the addition of the sulfur suspension separating agent, hydrophilic and hydrophobic groups can be effectively separated, and the problem of foam caused by two groups is solved. In addition, the sulfur suspension separating agent in the invention can not reduce the desulfurization efficiency of the adsorbent through detection, and the sulfur suspension separating agent has low cost and no obvious adverse environmental influence.

2. The sulfur suspension separating agent can be directly applied to a slurry bed, the regenerated sulfur-containing hydroxyl iron oxide does not need to be detached for separation treatment, and the sulfur suspension separating agent does not need to be taken out for separation operation after the adsorbent reaches the service life. Specifically, when the sulfur suspension separating agent is used, the sulfur suspension separating agent can be directly placed into a regeneration tank of a slurry bed, and the sulfur can be suspended and collected to the upper part of the liquid surface to form a sulfur floating foam layer with certain structural strength, so that the effect of floating partial sulfur can be achieved in the regeneration process of the adsorbent; because the sulfur amount wrapped on the surface of the adsorbent in the liquid is greatly reduced, part of covered active centers can be released, and the absorption efficiency of the hydrogen sulfide is improved; in addition, because the surface sulfur adsorption layer of the adsorbent to be regenerated is reduced, the regeneration effect is improved, so that the hydrogen sulfide adsorption effect of the regenerated adsorbent is improved to a certain extent; because the sulfur is concentrated on the upper part of the regeneration tank, the liquid at the middle lower part of the regeneration tank only needs to be directly returned to the absorption reactor of the slurry bed, and the aim of recycling is fulfilled. Meanwhile, the circulating amount of the sulfur-carrying solids is reduced in the liquid returned to the absorption reactor of the slurry bed, so that the pump force is saved, the abrasion to related parts is reduced, and the service life is prolonged.

Detailed Description

The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.