Recovery and dehydration treatment device for isooctyl p-nitrobenzoate and isooctyl alcohol

Abstract

The utility model relates to the field of chemical engineering, in particular to a device for recycling and dehydrating isooctyl p-nitrobenzoic acid isooctyl ester and isooctyl alcohol. The recovery and dehydration treatment device comprises a crude product tank, a desolventizing kettle, a dehydration kettle and a water storage tank which are sequentially connected, the desolventizing kettle is further connected with a finished product tank, the dehydration kettle is further connected with an isooctyl alcohol tank, a desolventizing water segregator is arranged between the desolventizing kettle and the dehydration kettle, and the water storage tank is connected with the desolventizing water segregator. A desolventizing condenser is arranged between the desolventizing water segregator and the desolventizing kettle, a dehydration water segregator is arranged between the dehydration kettle and the water storage tank, a dehydration condenser is arranged between the dehydration water segregator and the dehydration kettle, and a water pump is arranged between the water storage tank and the desolventizing kettle.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of chemical industry, concretely relates to a kind of recovery and dehydration treatment device of p-nitrobenzoic acid isooctyl ester isooctyl alcohol. BACKGROUND

[0002] Isooctyl alcohol is a colorless special smell flammable liquid, boiling point 183.5 ℃, insoluble in water, can be mutually soluble with most organic solvents. Its action is extensive, mainly used as solvent and preservative, also used as plastic main plasticizer and cold-resistant auxiliary plasticizer, defoaming agent, dispersing agent, ore dressing agent and petroleum additive, also used in printing and dyeing, paint, film etc.

[0003] Isooctyl alcohol is one of the main raw materials of p-nitrobenzoic acid isooctyl ester, in order to make the reaction quickly positive, excessive isooctyl alcohol is often used in industrial production, excessive amount is generally about 5%-10%, and downstream product requires content control to isooctyl alcohol, requires isoooctyl alcohol less than 0.2%, must remove isoooctyl alcohol, and for reducing cost, recycling of excessive isoooctyl alcohol is inevitable requirement. However, the isooctyl alcohol recovered generally recovers the way of azeotrope with water, so the isooctyl alcohol recovered contains more moisture, in order to reach use requirement when reusing, dehydration treatment to the isooctyl alcohol recovered is necessary. SUMMARY

[0004] The utility model discloses in order to solve the above-mentioned problems in prior art, in order to realize the efficiency of the recovery and dehydration treatment of p-nitrobenzoic acid isooctyl ester isooctyl alcohol and design. Its specific technical scheme is as follows:

[0005] A kind of recovery and dehydration treatment device of p-nitrobenzoic acid isooctyl ester isooctyl alcohol, including crude product tank that connects in turn, desolventizing kettle, dehydration kettle and water storage tank, the desolventizing kettle is also connected product tank, the dehydration kettle is also connected isooctyl alcohol tank, desolventizing kettle and dehydration kettle between being equipped with desolventizing water separator, desolventizing water separator and desolventizing kettle between being equipped with desolventizing condenser, dehydration kettle and water storage tank between being equipped with dehydration water separator, dehydration water separator and dehydration kettle between being equipped with dehydration condenser, water storage tank and desolventizing kettle between being equipped with water pump, crude product tank and desolventizing kettle between being equipped with crude product pump.

[0006] Crude product tank outlet valve is equipped on the crude product tank.

[0007] Desolventizing kettle includes desolventizing kettle feed valve, desolventizing kettle water inlet valve, desolventizing kettle gas phase outlet valve, desolventizing kettle reflux valve and desolventizing kettle bottom valve;Dehydration kettle includes dehydration kettle feed valve, dehydration kettle gas phase outlet valve, dehydration kettle reflux valve and dehydration kettle bottom valve.

[0008] Water storage tank includes water storage tank feed valve and water storage tank bottom valve;Product tank includes product tank feed valve and product tank bottom valve.

[0009] The isooctanol tank comprises an isooctanol tank feed valve and an isooctanol tank bottom valve; and the crude product pump comprises a crude product pump inlet valve and a crude product pump outlet valve.

[0010] The water pump comprises a water pump inlet valve and a water pump outlet valve.

[0011] The desolventizing water separator comprises a desolventizing water separator reflux port valve and a desolventizing water separator discharge port valve.

[0012] The dewatering water separator comprises a dewatering water separator reflux port valve and a dewatering water separator discharge port valve.

[0013] The utility model has the following advantages:

[0014] 1. The device can improve the recovery and dehydration treatment efficiency of isooctanol and p-nitrobenzoic acid isooctyl ester.

[0015] 2. The generated wastewater can be recycled and applied, and the pollution is small, which is friendly to the environment.

[0016] 3. The recovered isooctanol can be used to manufacture p-nitrobenzoic acid isooctyl ester. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 Figure 1 is a structural schematic diagram of the device for recovering and dehydrating isooctanol and p-nitrobenzoic acid isooctyl ester according to the utility model.

[0018] In the figure, 1 is a crude product tank; 101 is a crude product tank discharge valve; 2 is a desolventizing kettle; 201 is a desolventizing kettle feed valve; 202 is a desolventizing kettle water inlet valve; 203 is a desolventizing kettle gas phase outlet valve; 204 is a desolventizing kettle reflux valve; 205 is a desolventizing kettle bottom valve; 3 is a dewatering kettle; 301 is a dewatering kettle feed valve; 302 is a dewatering kettle gas phase outlet valve; 303 is a dewatering kettle reflux valve; 304 is a dewatering kettle bottom valve; 4 is a water storage tank; 401 is a water storage tank feed valve; 402 is a water storage tank bottom valve; 5 is a finished product tank; 501 is a finished product tank feed valve; 502 is a finished product tank bottom valve; 6 is an isooctanol tank; 601 is an isooctanol tank feed valve; 602 is an isooctanol tank bottom valve; 7 is a crude product pump; 701 is a crude product pump inlet valve; 702 is a crude product pump outlet valve; 8 is a water pump; 801 is a water pump inlet valve; 802 is a water pump outlet valve; 9 is a desolventizing water separator; 901 is a desolventizing water separator reflux port valve; 902 is a desolventizing water separator discharge port valve; 10 is a dewatering water separator; 1001 is a dewatering water separator reflux port valve; 1002 is a dewatering water separator discharge port valve; 11 is a desolventizing condenser; and 12 is a dewatering condenser. DETAILED DESCRIPTION

[0019] The device for recovering and dehydrating isooctanol and p-nitrobenzoic acid isooctyl ester according to the utility model will be further described below. Figure 1

[0020] ​The device for recovering and dehydrating isohexyl p-nitrobenzoate isohexanol, which comprises a crude product tank 1, a desolventizing kettle 2, a dehydration kettle 3 and a water storage tank 4 connected in sequence, the desolventizing kettle 2 is further connected to a finished product tank 5, the dehydration kettle 3 is further connected to an isohexanol tank 6, a desolventizing water separator 9 is arranged between the desolventizing kettle 2 and the dehydration kettle 3, a desolventizing condenser 11 is arranged between the desolventizing water separator 9 and the desolventizing kettle 2, a dehydration water separator 10 is arranged between the dehydration kettle 3 and the water storage tank 4, a dehydration condenser 12 is arranged between the dehydration water separator 10 and the dehydration kettle 3, a water pump 8 is arranged between the water storage tank 4 and the desolventizing kettle 2, and a crude product pump 7 is arranged between the crude product tank 1 and the desolventizing kettle 2.

[0021] The crude product tank 1 is provided with a crude product tank discharge valve 101.

[0022] The desolventizing kettle 2 comprises a desolventizing kettle feed valve 201, a desolventizing kettle water inlet valve 202, a desolventizing kettle gas phase outlet valve 203, a desolventizing kettle reflux valve 204 and a desolventizing kettle bottom valve 205.

[0023] The dehydration kettle 3 comprises a dehydration kettle feed valve 301, a dehydration kettle gas phase outlet valve 302, a dehydration kettle reflux valve 303 and a dehydration kettle bottom valve 304.

[0024] The water storage tank 4 comprises a water storage tank feed valve 401 and a water storage tank bottom valve 402.

[0025] The finished product tank 5 comprises a finished product tank feed valve 501 and a finished product tank bottom valve 502.

[0026] The isohexanol tank 6 comprises an isohexanol tank feed valve 601 and an isohexanol tank bottom valve 602; the crude product pump 7 comprises a crude product pump inlet valve 701 and a crude product pump outlet valve 702.

[0027] The water pump 8 comprises a water pump inlet valve 801 and a water pump outlet valve 802.

[0028] The desolventizing water separator 9 comprises a desolventizing water separator reflux port valve 901 and a desolventizing water separator discharge port valve 902.

[0029] The dehydration water separator 10 comprises a dehydration water separator reflux port valve 1001 and a dehydration water separator discharge port valve 1002.

[0030] The specific working process of the device is as follows:

[0031] 1, check whether the equipment is available according to the process flow before starting, all valves are in closed state, and confirm that there is no error.

[0032] 2、Preparation of crude, open crude tank 1 crude tank discharge valve 101, crude tank pump 7 crude tank pump inlet valve 701 and crude tank pump outlet valve 702, desolventizing kettle 2 desolventizing kettle feed valve 201, open crude tank pump 7, 4000 kg of crude from crude tank 1 into the desolventizing kettle 2 through the crude tank pump 7, after the end of the material, stop crude tank pump 7, close the crude tank discharge valve 101, crude tank pump inlet valve 701, crude tank pump outlet valve 702, desolventizing kettle feed valve 201.

[0033] 3、Add water, open desolventizing kettle 2 desolventizing kettle water inlet valve 202, water storage tank 4 water storage tank bottom valve 402, water pump 8 water pump inlet valve 801 and water pump outlet valve 802, open water pump 8, 400 kg of water from the water storage tank 4 into the desolventizing kettle 2 through the water pump 8, after the end of the material, stop water pump 8, close the water storage tank bottom valve 402, water pump inlet valve 801, water pump outlet valve 802, desolventizing kettle water inlet valve 202.

[0034] 3、Desolventizing, open desolventizing kettle 2 desolventizing kettle gas phase outlet valve 203, desolventizing kettle reflux valve 204 and desolventizing condenser 11 circulating water, start steam heating to 115℃, and keep the temperature, azeotropic reflux to remove isooctanol. Through the desolventizing water separator 9 sight glass observation, when the liquid in the desolventizing water separator 9 gradually increased, can be obviously found that there is a stratification phenomenon, the upper layer is isooctanol, the lower layer is water. When the amount of water gradually increased to 100 kg, open desolventizing water separator 9 to desolventizing kettle 2 desolventizing kettle reflux port valve 901, the water backflow to the desolventizing kettle 2, close the desolventizing water separator reflux port valve 901. After 20 h of continuous desolventizing, sample analysis, isooctanol content is 0.15%, qualified, desolventizing end. Start cooling, desolventizing kettle 2 kettle temperature to 30℃, open desolventizing kettle 2 desolventizing kettle bottom valve 205 and product tank 5 product tank feed valve 501, the material from the desolventizing kettle 2 into the product tank 5, can be used for downstream product production, after closing the desolventizing kettle bottom valve 205 and product tank feed valve 501. Open desolventizing water separator 9 to desolventizing kettle 3 desolventizing water separator discharge port valve 902 and desolventizing kettle 3 desolventizing kettle feed valve 301, isooctanol (about 250 kg) into the desolventizing kettle 3, close the desolventizing water separator discharge port valve 902, desolventizing kettle feed valve 301. Open desolventizing water separator 9 to desolventizing kettle 2 desolventizing water separator reflux port valve 901, the water backflow to the desolventizing kettle 2, close the desolventizing water separator reflux port valve 901, while recording the liquid level amount is 365 kg, open desolventizing kettle water inlet valve 202, add 35 kg of water, for the next batch of desolventizing.

[0035] 4、dehydration, dehydration kettle 3 in the collection 10 batches (about 2500kg) of isooctanol, open dehydration kettle gas phase export valve 302, dehydration kettle reflux valve 303, dehydration water separator 10 dehydration water separator reflux port valve 1001 and dehydration condenser 12 circulating water, start steam heating to 105℃, and keep the temperature, azeotropic dehydration. Continuous dehydration 5h, sampling analysis, moisture content of 0.12%, qualified, dehydration end. Start cooling, dehydration kettle 3 kettle temperature to 30℃, open the dehydration kettle 3 dehydration kettle bottom valve 304 and isooctanol tank 6 isooctanol tank feed valve 601, isooctanol from dehydration kettle 2 into isooctanol tank 6, can be used for p-nitrobenzoic acid isooctyl ester production, after closing the dehydration kettle bottom valve 304 and isooctanol tank feed valve 601. Open dehydration water separator 10 to water storage tank 4 on the dehydration water separator discharge port valve 1002 and water storage tank 4 on the water storage tank feed valve 401, about 350kg of water layer into the water storage tank 4 after, can be used for desolventization, close the dehydration water separator discharge port valve 1002 and water storage tank feed valve 401.

[0036] Finally, it should be noted that: the above examples are used to illustrate the technical scheme of the present application, rather than limit it; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that: it can still modify the technical scheme recorded in the foregoing examples, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical scheme deviate from the scope of the technical scheme of the embodiments of the present application.

Claims

1. A device for the recovery and dehydration of isooctyl p-nitrobenzoate with isooctanol, characterized by the fact that it comprises: The crude product tank, the desolventizing kettle, the dehydration kettle and the water storage tank are connected in sequence, the desolventizing kettle is further connected to the finished product tank, the dehydration kettle is further connected to the isooctanol tank, a desolventizing water separator is arranged between the desolventizing kettle and the dehydration kettle, a desolventizing condenser is arranged between the desolventizing water separator and the desolventizing kettle, a dehydration water separator is arranged between the dehydration kettle and the water storage tank, a dehydration condenser is arranged between the dehydration water separator and the dehydration kettle, a water pump is arranged between the water storage tank and the desolventizing kettle, and a crude product pump is arranged between the crude product tank and the desolventizing kettle.

2. A device for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol according to claim 1, characterized in that: The crude product tank is provided with a crude product tank discharge valve.

3. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1, wherein: The desolventizing kettle comprises a desolventizing kettle feed valve, a desolventizing kettle water inlet valve, a desolventizing kettle gas phase outlet valve, a desolventizing kettle reflux valve and a desolventizing kettle bottom valve; and the dehydration kettle comprises a dehydration kettle feed valve, a dehydration kettle gas phase outlet valve, a dehydration kettle reflux valve and a dehydration kettle bottom valve.

4. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1, wherein: The water storage tank comprises a water storage tank feed valve and a water storage tank bottom valve; and the finished product tank comprises a finished product tank feed valve and a finished product tank bottom valve.

5. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1, wherein: The isooctanol tank comprises an isooctanol tank feed valve and an isooctanol tank bottom valve; and the crude product pump comprises a crude product pump inlet valve and a crude product pump outlet valve.

6. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1 wherein: The water pump comprises a water pump inlet valve and a water pump outlet valve.

7. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1 wherein: The desolventizing water separator comprises a desolventizing water separator reflux port valve and a desolventizing water separator discharge port valve.

8. A process for recovery and dehydration of isooctyl p-nitrobenzoate and isooctanol as claimed in claim 1, wherein: The dehydration water separator comprises a dehydration water separator reflux port valve and a dehydration water separator discharge port valve.

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