阅读说明：本技术 一种活性二氯化硫制备工艺 (Preparation process of active sulfur dichloride ) 是由 宗广斌 于 2019-10-14 设计创作，主要内容包括：本发明公开了一种活性二氯化硫制备工艺,涉及二氯化硫制备技术领域,为解决现有的活性二氯化硫生产制备完成后会产生极大的污染性气体,臭味十分浓烈,不能很好的得到处理,影响后期使用,且二氯化硫的生产制备性能还不够完善的问题。步骤1：一氯化硫初反应加热,将一氯化硫加入夹层反应器中,通入蒸汽进行加热；步骤2：加入氯气,此时夹层反应器内部温度设置为100-110℃,氯气加入反应6h,通氯气量设置为75L/h,氯气完全反应后,即可停止通氯气；步骤3：加入三氯化磷稳定剂混合；步骤4：预热蒸馏除去氯气；步骤5：除臭处理。(The invention discloses a preparation process of active sulfur dichloride, relates to the technical field of sulfur dichloride preparation, and aims to solve the problems that after the existing active sulfur dichloride is produced and prepared, extremely polluting gas is generated, the odor is very strong, the active sulfur dichloride cannot be well treated, the later use is influenced, and the production and preparation performance of the sulfur dichloride is not complete. Step 1: heating the sulfur monochloride through a primary reaction, adding the sulfur monochloride into an interlayer reactor, and introducing steam for heating; step 2: adding chlorine, wherein the internal temperature of the sandwich reactor is set to be 100-; and step 3: adding a phosphorus trichloride stabilizer and mixing; and 4, step 4: preheating and distilling to remove chlorine; and 5: and (5) deodorizing.)

1. A preparation process of active sulfur dichloride is characterized by comprising the following steps: the method comprises the following steps:

step 1: heating the sulfur monochloride through a primary reaction, adding the sulfur monochloride into a sandwich reactor, introducing steam for heating, carrying a gas mask by an operator, and carrying out the primary reaction heating on the sulfur monochloride to carry out the next preparation;

step 2: adding chlorine, wherein the internal temperature of the sandwich reactor is set to be 100-;

and step 3: adding a phosphorus trichloride stabilizer for mixing, adding the phosphorus trichloride stabilizer into the interlayer reactor, starting a stirring rod in the reactor after adding the phosphorus trichloride stabilizer, and stirring the inside to uniformly mix the inside;

and 4, step 4: preheating and distilling to remove chlorine, starting a heater in the interlayer reactor, taking out the prepared sulfur dichloride after the chlorine in the interlayer reactor is removed, and filling the sulfur dichloride in a sealed anti-corrosion container so as to facilitate the next preparation treatment;

and 5: and (2) deodorizing, namely adding sulfur dichloride into a reaction tower, filling a special solid composite filler in the reaction tower, compounding a multi-medium catalyst in the filler, fully contacting a liquid-phase compound oxidant sprayed out in a divergent mist shape through a stop nozzle after malodorous gas passes through the filler layer under the action of an induced draft fan on the surface of the solid filler, fully decomposing pollution factors in the malodorous gas under the catalytic action of the multi-medium catalyst, and performing the next processing treatment after decomposition.

2. The process according to claim 1, characterized in that: the heating temperature in the interlayer reactor in the step 1 is set to be 90-100 ℃, and the heating time is set to be 20-40 min.

3. The process according to claim 1, characterized in that: the dosage of the stabilizer phosphorus trichloride added in the step 3 is set to be 0.1-0.25%.

4. The process according to claim 1, characterized in that: and 4, heating the internal temperature of the reactor to 60-63 ℃ for 1-2 h.

5. The process according to claim 1, characterized in that: in the step 4, a chlorine detector can be used to detect whether chlorine is completely removed.

6. The process according to claim 1, characterized in that: and 5, setting the time of the deodorization treatment in the step 5 to be 4h, and collecting sulfur dichloride after the deodorization treatment by adopting a special anti-corrosion container.

7. The process according to claim 1, characterized in that: and 3, setting the stirring time of the stirring device in the step 3 to be 2-3h, and stirring for 2-3h to enable the phosphorus trichloride stabilizer to be mixed and fully mixed with the liquid in the phosphorus trichloride stabilizer.

8. The process according to claim 1, characterized in that: in the step 5, the solid composite filler needs to be replaced properly as the service life increases, and needs to be replaced after the deodorization treatment is carried out for three to five times.

Technical Field

The invention relates to the technical field of sulfur dichloride preparation, in particular to a preparation process of active sulfur dichloride.

Background

Sulfur dichloride, dark red or light red liquid, has pungent odor, dissolves in water and reacts violently, has strong irritation to eye and upper respiratory mucosa, and can cause severe skin burn. Less serious patients can cause pulmonary edema, sulfur dichloride is an intermediate for preparing carbamate insecticides, namely carbosulfan and benfuracarb, can also be used as an organically synthesized chlorinating agent, for preparing acid anhydride or chloride of organic acid, high-pressure lubricating oil, can be used as an additive of cutting oil, a processing agent for processing vegetable oil (such as corn oil, cottonseed oil and soybean oil) in the oil industry, and also can be used as a disinfectant and a bactericide.

However, after the existing active sulfur dichloride is produced and prepared, extremely polluted gas can be generated, the odor is very strong, the active sulfur dichloride cannot be well treated, the later-stage use is influenced, and the production and preparation performance of the sulfur dichloride is not perfect; therefore, the existing requirements are not met, and an active sulfur dichloride preparation process is provided for the process.

Disclosure of Invention

The invention aims to provide a preparation process of active sulfur dichloride, which aims to solve the problems that the existing preparation process of the active sulfur dichloride in the background art can generate extremely polluted gas after the production is finished, the odor is very strong, the active sulfur dichloride cannot be well treated, the later use is influenced, and the production and preparation performance of the sulfur dichloride is not complete.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation process of active sulfur dichloride comprises the following steps:

step 1: heating the sulfur monochloride through a primary reaction, adding the sulfur monochloride into a sandwich reactor, introducing steam for heating, carrying a gas mask by an operator, and carrying out the primary reaction heating on the sulfur monochloride to carry out the next preparation;

step 2: adding chlorine, wherein the internal temperature of the sandwich reactor is set to be 100-;

and step 3: adding a phosphorus trichloride stabilizer for mixing, adding the phosphorus trichloride stabilizer into the interlayer reactor, starting a stirring rod in the reactor after adding the phosphorus trichloride stabilizer, and stirring the inside to uniformly mix the inside;

and 4, step 4: preheating and distilling to remove chlorine, starting a heater in the interlayer reactor, taking out the prepared sulfur dichloride after the chlorine in the interlayer reactor is removed, and filling the sulfur dichloride in a sealed anti-corrosion container so as to facilitate the next preparation treatment;

and 5: and (2) deodorizing, namely adding sulfur dichloride into a reaction tower, filling a special solid composite filler in the reaction tower, compounding a multi-medium catalyst in the filler, fully contacting a liquid-phase compound oxidant sprayed out in a divergent mist shape through a stop nozzle after malodorous gas passes through the filler layer under the action of an induced draft fan on the surface of the solid filler, fully decomposing pollution factors in the malodorous gas under the catalytic action of the multi-medium catalyst, and performing the next processing treatment after decomposition.

Preferably, the heating temperature in the step 1 sandwich reactor is set to be 90-100 ℃, and the heating time is set to be 20-40 min.

Preferably, the amount of the stabilizer phosphorus trichloride added in the step 3 is set to be 0.1-0.25%.

Preferably, the step 4 heats the temperature inside the reactor to 60-63 ℃ for 1-2 h.

Preferably, a chlorine detector may be used in step 4 to detect whether chlorine is completely removed.

Preferably, the time of the deodorization treatment in the step 5 is set to be 4 hours, and a special anti-corrosion container is adopted for collecting sulfur dichloride after the deodorization treatment is finished.

Preferably, the stirring time of the stirring device in the step 3 is set to be 2-3h, and the phosphorus trichloride stabilizer can be mixed with the liquid in the phosphorus trichloride stabilizer to be fully mixed after stirring for 2-3 h.

Preferably, the solid composite filler in the step 5 needs to be replaced appropriately as the service life increases, and needs to be replaced after the deodorization treatment is performed three to five times.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, the deodorization treatment is carried out after the sulfur dichloride is processed, so that the later-stage processing service performance of the sulfur dichloride is more perfect, the influence of too odor on the environment is avoided, and the problems that the existing active sulfur dichloride can generate extremely polluted gas after being produced and prepared, the odor is very strong, the treatment cannot be well carried out, and the later-stage use is influenced are solved.

2. According to the invention, when the chlorine gas is added, the internal temperature of the sandwich reactor is set to be 100-.

Drawings

FIG. 1 is a process flow diagram of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

Referring to fig. 1, an embodiment of the present invention: a preparation process of active sulfur dichloride comprises the following steps:

step 1: heating the sulfur monochloride through a primary reaction, adding the sulfur monochloride into a sandwich reactor, introducing steam for heating, carrying a gas mask by an operator, and carrying out the primary reaction heating on the sulfur monochloride to carry out the next preparation;

step 2: adding chlorine, wherein the internal temperature of the sandwich reactor is set to be 100-;

and step 3: adding a phosphorus trichloride stabilizer for mixing, adding the phosphorus trichloride stabilizer into the interlayer reactor, starting a stirring rod in the reactor after adding the phosphorus trichloride stabilizer, and stirring the inside to uniformly mix the inside;

and 4, step 4: preheating and distilling to remove chlorine, starting a heater in the interlayer reactor, taking out the prepared sulfur dichloride after the chlorine in the interlayer reactor is removed, and filling the sulfur dichloride in a sealed anti-corrosion container so as to facilitate the next preparation treatment;

and 5: and (2) deodorizing, namely adding sulfur dichloride into a reaction tower, filling a special solid composite filler in the reaction tower, compounding a multi-medium catalyst in the filler, fully contacting a liquid-phase compound oxidant sprayed out in a divergent mist shape through a stop nozzle after malodorous gas passes through the filler layer under the action of an induced draft fan on the surface of the solid filler, fully decomposing pollution factors in the malodorous gas under the catalytic action of the multi-medium catalyst, and performing the next processing treatment after decomposition.

Further, the heating temperature in the sandwich reactor in the step 1 is set to be 90-100 ℃, and the heating time is set to be 20-40 min.

Further, the dosage of the stabilizer phosphorus trichloride added in the step 3 is set to be 0.1-0.25%.

Further, step 4, heating the internal temperature of the reactor to 60-63 ℃ for 1-2 h.

Further, in step 4, a chlorine detector may be used to detect whether chlorine is completely removed.

Further, the time of the deodorization treatment in the step 5 is set to be 4 hours, and a special anti-corrosion container is adopted for collection when the sulfur dichloride is taken out after the deodorization treatment is finished.

Further, the stirring time of the stirring device in the step 3 is set to be 2-3 hours, and the phosphorus trichloride stabilizer can be mixed with the liquid in the phosphorus trichloride stabilizer and fully mixed by stirring for 2-3 hours.

Further, the solid composite packing in step 5 needs to be appropriately replaced as the use time increases, and needs to be replaced after three to five times of deodorization treatment.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.