CN107312562B

CN107312562B - Refining system and process for refining wood vinegar by using wood raw materials

Info

Publication number: CN107312562B
Application number: CN201710572777.9A
Authority: CN
Inventors: 王玉东
Original assignee: Shandong Dongmeng Biotechnology Development Co ltd
Current assignee: Shandong Dongmeng Biotechnology Development Co ltd
Priority date: 2017-07-13
Filing date: 2017-07-13
Publication date: 2023-04-21
Anticipated expiration: 2037-07-13
Also published as: CN107312562A

Abstract

The invention discloses a refining system for refining wood vinegar by using wood raw materials and a process thereof, wherein the process comprises the following steps: step 1, putting wood raw materials into a crushing device for crushing, starting a heating device, and putting the crushed wood raw materials into a distillation furnace; step 2, distillation is divided into three stages, namely first stage distillation, second stage distillation and third stage distillation; and 3, separating. The system comprises: the wood vinegar separating device comprises a feeding system, a plurality of wood vinegar distilling systems and a wood vinegar separating system. The invention can effectively remove the moisture and tar components of the crude pyroligneous liquor, and has the advantages of stable effective components, strong oxidation resistance, high content of effective components and strong antibacterial effect.

Description

Refining system and process for refining wood vinegar by using wood raw materials

Technical Field

The invention belongs to the field of fine chemicals, and particularly relates to a refining system and a process for refining wood vinegar by using wood raw materials.

Background

The wood vinegar is a natural extract prepared by fractionating flue gas in the pyrolysis distillation process of wood materials, and is a system substance with complex components, multiple functions and relative stability. The wood vinegar is generally light brown to dark brown semitransparent liquid, has unique smoke fragrance, is sour, has a PH value of 1.5-3.7 and has a specific gravity of 1.0025; it contains more than 200 organic matters including phenols, acids, alcohols, ketones, etc., and has complex components, various functions and natural balance of various trace substance factors.

The wood vinegar has various bioactive functions and is widely applied to agriculture, forestry, animal husbandry, food processing industry, medical and health industry and light industry; but also has a plurality of magic effects in practical application. In agriculture, the wood vinegar is a good green fertilizer and pesticide, and the mixture of various organic matters contained in the wood vinegar has various functions of promoting plant growth, soil disinfection, sterilization, insect prevention, corrosion prevention, weeding, deodorization and the like, can be used as a micro-fertilizer, improves crop yield and quality, and is widely applied to agriculture. In medical aspect, the refined wood vinegar can be used as an additive component of medicines and cosmetics, and has curative effects on atopic dermatitis, eczema and wound. In recent years, along with consumer's disfigurement of natural plant source extracts, wood vinegar is used as one of green natural plant source bacteriostats, and the demand of the international market for wood vinegar is increasing dramatically.

At present, few manufacturers specially producing wood vinegar in China. Although wood vinegar can be used as a good byproduct in the charcoal production industry, common charcoal manufacturers often discharge flue gas into the air during charcoal production, and wood vinegar is not fractionated and recovered; even if some charcoal manufacturers recover, they do not collect and refine them efficiently. On the other hand, the flue gas generated during the charcoal firing process is widely discharged into the air, wherein CO, NO, etc. generated by incomplete combustion seriously pollute the environment.

The apricot shell is obtained by breaking mature seed of Prunus armeniaca or Prunus Arnica of Prunaceae. The apricot shell is dense and tough, and pyrolysed to obtain the wood vinegar. The Chinese patent (200710011840.8) with publication number 101074382A discloses a process for extracting pyroligneous liquor from apricot shells, wherein the apricot shells are added into a carbonization kettle, air pyrolysis is isolated for 4-6 hours at 450-550 ℃, gas phase products led out from the carbonization kettle are condensed, and a condensable part is taken to obtain crude pyroligneous liquor; standing the crude pyroligneous liquor for more than 30 days, separating 3 layers, rectifying the middle layer at 90-120 ℃ for 4-6 hours, and condensing to obtain the refined pyroligneous liquor product.

The disclosure of the above patent discloses a technical scheme of providing refined pyroligneous liquor by using apricot shells as original pyrolysis, but the whole process is time-consuming and laborious, especially the refined part of pyroligneous liquor is firstly stood for 30 days, and after layering, the refined part is heated and refined by using traditional pyroligneous liquor, so that the manufacturing efficiency is greatly slowed down and delayed; one of the great advantages of pyroligneous liquor is the comprehensive balance of various organic components, the middle layer is reserved for rectification after standing, and the organic components contained in the upper layer and the lower layer which are discarded are wasted. In addition, the energy consumption in the wood vinegar production process is also relatively high.

Disclosure of Invention

The invention aims to solve the problems in the prior art and aims to design and provide a refining system for refining wood vinegar by using wood raw materials and a process thereof.

The technical scheme adopted by the invention is as follows.

A refining system for refining wood vinegar from wood raw materials, comprising: the wood vinegar separating device comprises a feeding system, a plurality of wood vinegar distilling systems and a wood vinegar separating system.

The feed system includes a comminution device.

The wood vinegar distillation system comprises a distillation furnace, a heating device and a gas auxiliary heating device.

The wood vinegar separating system comprises a condenser sealing and standing separating device, a standing separating device and a water sealing device; the side wall of the sealing and standing separation device is provided with a sealing and standing separation device side valve, and the bottom of the sealing and standing separation device is provided with a sealing and standing separation device bottom valve; a side valve of the static separation device is arranged on the side wall of the static separation device, and a bottom valve of the static separation device is arranged at the bottom of the static separation device; the top of the distillation furnace is connected with a condenser through a pipeline, and the condenser is connected with a sealed static separation device through a pipeline; the top of the sealed static separation device is connected with a water sealing device through a pipeline, and the water sealing device is connected with at least one gas auxiliary heating device of the wood vinegar distillation system through a pipeline; the bottom valve of the sealed static separation device is connected with at least one distillation furnace of the wood vinegar distillation system through a pipeline; the valve at the side of the sealed static separation device is connected with the static separation device through a pipeline; a vacuum pump is arranged on a pipeline between the water sealing device and the sealing standing separation device; a pipeline at the top of the distillation furnace is provided with a distillation furnace pressure control valve; the top of the static separation device is provided with an opening.

As a preferable technical scheme, the number of the wood vinegar distillation systems is 1-6; the wood vinegar separating system also comprises a wood tar storage device and a wood vinegar storage device, and a bottom valve of the standing separating device is connected with the wood tar storage device through a pipeline; the valve at the side of the standing separation device is connected with the pyroligneous liquor storage device through a pipeline.

As a preferable technical scheme, the side wall of the static separation device is provided with a liquid outlet hole; the side valve of the static separation device comprises a floating plate valve capable of sealing a liquid outlet hole on the side wall of the static separation device, a floating plate valve supporting spring and a floating plate valve horizontal limiting vertical plate arranged on the bottom surface of the static separation device, when the liquid in the static separation device is smaller than or equal to a certain density, the floating plate valve descends under the action of buoyancy and gravity and seals the liquid outlet hole on the side wall of the static separation device, when the liquid in the static separation device is larger than the certain density, the floating plate valve floats upwards under the action of the buoyancy and the floating plate valve supporting spring and does not seal the liquid outlet hole on the side wall of the static separation device, the floating plate valve is positioned between the side wall of the liquid outlet hole of the static separation device and the floating plate valve horizontal limiting vertical plate and is contacted with the side wall of the liquid outlet hole and the floating plate valve horizontal limiting vertical plate, and a plurality of through holes are horizontally arranged on the floating plate valve.

The bottom surface of the static separation device is provided with a bottom liquid outlet hole, the bottom valve of the static separation device comprises a floating valve arranged on the bottom liquid outlet hole of the bottom surface of the static separation device, the bottom surface of the floating valve is provided with an inserting rod which is inserted into the bottom liquid outlet hole of the bottom surface of the static separation device, and the diameter of the inserting rod is slightly smaller than that of the bottom liquid outlet hole of the bottom surface of the static separation device; when the liquid at the bottom of the static separation device is greater than a certain density, the floating valve is separated from the bottom liquid outlet hole under the action of the floating force, the liquid at the bottom of the static separation device flows out from the bottom liquid outlet hole, and when the liquid at the bottom of the static separation device is less than a certain density, the floating valve is contacted with the bottom liquid outlet hole under the neutral effect, so that the liquid at the bottom of the static separation device is prevented from flowing out from the bottom liquid outlet hole.

As a preferable technical scheme, the wood vinegar separating system comprises a negative pressure sealing and standing separating device, wherein the negative pressure sealing and standing separating device is arranged on a pipeline between a valve at the side of the sealing and standing separating device and the standing separating device; the side wall of the negative pressure sealing and standing separation device is provided with a negative pressure sealing and standing separation device side valve, and the bottom of the negative pressure sealing and standing separation device is provided with a negative pressure sealing and standing separation device bottom valve; the negative pressure sealing static separation device side valve is connected with the static separation device through a pipeline, and the negative pressure sealing static separation device bottom valve is communicated with a pipeline between the sealing static separation device bottom valve and the distillation furnace through a pipeline; the top of the negative pressure sealing static separation device is connected with a low pressure water seal device through a pipeline, and the low pressure water seal device is connected with a pipeline between the water seal device and the gas auxiliary heating device through a pipeline; a vacuum pump of the negative pressure sealing static separation device is arranged on a pipeline between the low pressure water sealing device and the negative pressure sealing static separation device.

As the preferable technical scheme, the wood vinegar separating system further comprises an activated carbon adsorption device, and a valve at the side of the standing separating device is connected with the activated carbon adsorption device through a pipeline.

As a preferable technical scheme, the distillation furnace is provided with a charcoal discharge port, the wood vinegar separating system also comprises a steam activating device, and the steam activating device comprises a heating device; the water sealing device is connected with the heating device of the steam activating device through a pipeline.

A process for refining wood vinegar by adopting the refining system comprises the following steps:

step 1: crushing wood raw materials in a crushing device, starting a heating device, and putting the crushed wood raw materials in a distillation furnace; the wood raw material is the branch of a fruit tree;

step 2: the distillation fraction is divided into three stages, namely a first stage distillation, a second stage distillation and a third stage distillation.

First stage distillation

The distillation temperature is controlled at 95-135 ℃ and the distillation time is 1-3h, flue gas in the distillation furnace is led into a condenser, liquid formed after the flue gas is condensed is led into a sealed static separation device, a vacuum pump is started, gas volatilized from the liquid in the sealed static separation device is led into a water sealing device and is led into a gas auxiliary heating device through a pipeline for combustion; after the first-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device into a distillation furnace, and introducing the rest liquid in the sealed static separation device into the static separation device.

Second stage distillation

The distillation temperature is controlled at 136-280 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.5-2.0 atm, the pressure control valve of the distillation furnace is started, flue gas in the distillation furnace is led into a condenser, liquid formed after the flue gas is condensed is led into a sealed static separation device, a vacuum pump is started, and gas volatilized from the liquid in the sealed static separation device is led into a water sealing device and is led into a gas auxiliary heating device through a pipeline for combustion; and after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device into a distillation furnace, and introducing the rest liquid in the sealed static separation device into the static separation device.

Third stage distillation

The distillation temperature is controlled to 281-350 ℃, the distillation time is 3-5h, when the pressure in the distillation furnace is 1.5-2.5 atm, the pressure control valve of the distillation furnace is started, the flue gas in the distillation furnace is led into the condenser, the liquid formed after the flue gas is condensed is led into the sealed static separation device, the vacuum pump is started, and the gas volatilized from the liquid in the sealed static separation device is led into the water sealing device and is led into the gas auxiliary heating device for combustion through the pipeline; and after the third-stage distillation is finished, introducing all liquid in the sealed static separation device into a distillation furnace.

Step 3: separation

And (3) standing all the liquid in the standing separation device for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device, discharging the liquid at the bottom from a bottom valve of the standing separation device, and then discharging the solution from a side valve of the standing separation device to obtain the pyroligneous liquor.

step 1: crushing wood raw materials in a crushing device, starting a heating device, and putting the crushed wood raw materials in a distillation furnace;

First stage distillation

The distillation temperature is controlled at 95-135 ℃ and the distillation time is 1-3h, flue gas in the distillation furnace is led into a condenser, liquid formed after the flue gas is condensed is led into a sealed static separation device, a vacuum pump is started, gas volatilized from the liquid in the sealed static separation device is led into a water sealing device and is led into a gas auxiliary heating device through a pipeline for combustion; after the first-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device into a distillation furnace, and introducing the rest liquid in the sealed static separation device into the negative pressure sealed static separation device.

Second stage distillation

The distillation temperature is controlled at 136-280 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.5-2.0 atm, the pressure control valve of the distillation furnace is started, flue gas in the distillation furnace is led into a condenser, liquid formed after the flue gas is condensed is led into a sealed static separation device, a vacuum pump is started, and gas volatilized from the liquid in the sealed static separation device is led into a water sealing device and is led into a gas auxiliary heating device through a pipeline for combustion; and after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device into a distillation furnace, and introducing the rest liquid in the sealed static separation device into the negative pressure sealed static separation device.

Third stage distillation

Step 3: separation

A step of low-pressure static separation in a negative-pressure sealed static separation device, wherein the static time is 1-2h; when the pressure in the negative pressure sealing and standing separation device is 1.2-1.5 atmospheres, starting a vacuum pump of the negative pressure sealing and standing separation device, and introducing smoke in the negative pressure sealing and standing separation device into a low-pressure water seal device and a gas auxiliary heating device through a pipeline for combustion; after the low-pressure static separation is finished, introducing liquid at the bottom of the negative pressure sealing static separation device into a distillation furnace, and introducing the rest liquid in the negative pressure sealing static separation device into the static separation device;

First stage distillation

Second stage distillation

Third stage distillation

Step 3: separation

Standing all the liquid in a standing separation device for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device, discharging the liquid at the bottom from a bottom valve of the standing separation device, and then placing the solution discharged from a side valve of the standing separation device into an activated carbon adsorption device for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar.

step 1: the wooden raw materials are put into a crushing device for crushing, a heating device is started, and the crushed wooden raw materials are put into a distillation furnace.

First stage distillation

Second stage distillation

Third stage distillation

Step 3: separation

Standing all the liquid in a standing separation device for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device, discharging the liquid at the bottom from a bottom valve of the standing separation device, and then placing the solution discharged from a side valve of the standing separation device into an activated carbon adsorption device for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar; the preparation method of the activated carbon comprises the steps of taking charcoal out from a charcoal discharge hole of a distillation furnace, and then putting the charcoal into a steam activating device, wherein fuel gas of a heating device of the steam activating device is from a water sealing device.

Compared with the prior art, the invention has the following technical effects.

1. The invention provides a system and a process for extracting wood vinegar by using wood raw materials, which comprise a preparation method of wood vinegar by using wood raw materials, and can also produce wood tar, the production process is simple, the product effect is good, the added value of the wood raw materials is greatly improved, the utilization of forestry resources in China is improved, and the formation of forestry industrialization is promoted. The wood raw materials are preferably fruit tree branches, a large number of fruit trees need to be pruned every year in China, a large number of fruit tree branches are generated, and the raw materials are superior raw materials for producing wood vinegar, but are generally burnt. These products can be effectively utilized by the method of the present invention.

2. The preparation method of the pyroligneous liquor has the advantages of simple and environment-friendly production process, high production efficiency, and accurate control of the effective components of the pyroligneous liquor through three times of distillation under different pressure conditions and standing separation under different pressure conditions; and finally, standing separation is carried out under the condition of no pressure, and the standing separation under the condition of no pressure is slowly completed in the system, so that the method is very efficient. The whole process is continuous and time-consuming, and can be refined to obtain refined wood vinegar; because the moisture and tar components of the crude pyroligneous are effectively removed, the natural plant source bacteriostatic agent which can be applied to agriculture and medicine is obtained, and the natural plant source bacteriostatic agent has the advantages of stable active ingredients, strong oxidation resistance, high active ingredient content and strong bacteriostatic effect. The experiment result shows that the wood vinegar produced by the process of the invention contains acetic acid as main component, the relative content of acetic acid is 50.3-51.2%, and 18 kinds of 45-62 kinds of components such as alcohols, esters, ketones, phenols, etc. The color of the wood vinegar produced by the invention is light yellow brown or light red brown in examples 1-9, the liquid produced by examples 10 and 11 is light brown, the natural wood vinegar contains more than 200 components, 45-52 components of the wood vinegar produced by the invention indicate that some components which are easy to oxidize and change are separated. The small amount of wood vinegar dipped in each embodiment is dripped on white paper, and after the wood vinegar is dried, the wood vinegar is observed to be light brown transparent liquid, and no black or black brown liquid stain appears on one side, which indicates that the wood vinegar is relatively stable and is not easy to be oxidized by oxygen in the air or generate photochemical reaction. And placing the produced pyroligneous liquor into a test tube for standing for 5 minutes, wherein suspended matters are not generated, which indicates that the pyroligneous liquor has good quality.

3. The water sealing device is arranged, so that tempering can be effectively prevented, and the water sealing device is safer.

4. The whole process is very environment-friendly and does not release smoke. In the preferred system, active carbon generated by the system is also adopted to adsorb pyroligneous liquor, so that the pyroligneous liquor has good extraction effect, and the internal circulation of products and energy is realized. The iodine adsorption value of the obtained wood raw material active carbon is 1125mg/g, the methylene blue adsorption value is 170mg/g, and the wood raw material active carbon has strong adsorption capacity, large toughness and stable chemical property. The social, environmental protection and economic benefits are very outstanding.

5. The whole system is very energy-saving and efficient, and the high-density liquid at the bottom of the sealed static separation device is added into the distillation furnace again for repeated distillation, so that the decomposition is thorough.

6. The whole system is very energy-saving, all the generated waste gas is used for auxiliary combustion, and according to experiments, the distillation furnace has 80-83% of combustion energy derived from the waste gas generated by production, in the production, only the first stage distillation needs the heating device to operate in advance, and the gas generated in the later stage can be fully supplied to the gas auxiliary heating device for use, and the heat generated by the heating device is only used as a supplement. The wood vinegar prepared by the method has the advantages of complete retention of active ingredients, multiple functions, simple and environment-friendly preparation method, low energy consumption and high production efficiency.

Drawings

FIG. 1 is a schematic diagram of a system for extracting wood vinegar from wood materials according to a preferred embodiment of the present invention.

Fig. 2 is a schematic structural diagram of a system for refining wood vinegar by using wood materials according to a preferred embodiment of the present invention.

Fig. 3 is a schematic structural diagram of a system for refining wood vinegar by using wood materials according to a preferred embodiment of the present invention.

Fig. 4 is a schematic structural diagram of a system for refining wood vinegar by using wood materials according to a preferred embodiment of the present invention.

Fig. 5 is a schematic structural view of the stationary separation apparatus.

Wherein: a wood vinegar distillation system-1; wood vinegar separating system-2; a feeding system-3; a crushing device-4; a distillation furnace-5; charcoal discharge port-51; a distillation furnace pressure control valve-52; a heating device-6; a gas auxiliary heating device-7; a condenser-8; sealing and standing a separating device-9; sealing and standing a valve-91 at the side of the separation device; sealing and standing a bottom valve-92 of the separation device; a first liquid density measuring device-93; standing and separating device-10; standing a valve-101 at the side of the separation device; standing a bottom valve-102 of the separation device; an opening-103; a second liquid density measuring device-104; a through-hole-105; a liquid outlet hole-106; a floating plate valve-107; a floating plate valve supporting spring-108; a plate horizontal limit vertical plate-109; bottom outlet hole-1010; a float valve-1011; insert bar-1012; a water seal device-11; a wood tar storage device-12; wood vinegar storage device-13; activated carbon adsorption means-131; a water vapor activation device-132; a vacuum pump-14; negative pressure sealing and standing separation device-15; negative pressure sealing and standing separation device side valve-151; negative pressure sealing and standing separation device bottom valve-152; vacuum pump-16 of negative pressure sealing static separation device; low-pressure water seal device-17.

Detailed Description

The invention will now be further described with reference to the drawings and examples.

Example 1. As shown in fig. 1, a refining system for refining wood vinegar by using wood materials, comprising: a feeding system 3, a wood vinegar distillation system 1 and a wood vinegar separation system 2;

the feeding system 3 comprises a crushing device 4;

the wood vinegar distillation system 1 comprises a distillation furnace 5, a heating device 6 and a gas auxiliary heating device 7;

the wood vinegar separating system 2 comprises a condenser 8, a sealed static separation device 9, a static separation device 10 and a water seal device 11; a side valve 91 of the sealing and standing separation device is arranged on the side wall of the sealing and standing separation device 9, and a bottom valve 92 of the sealing and standing separation device is arranged at the bottom of the sealing and standing separation device 9; a valve 101 at the side of the static separation device is arranged on the side wall of the static separation device 10, and a valve 102 at the bottom of the static separation device 10 is arranged at the bottom of the static separation device; the top of the distillation furnace 5 is connected with a condenser 8 through a pipeline, and the condenser 8 is connected with a sealed static separation device 9 through a pipeline; the top of the sealed static separation device 9 is connected with a water seal device 11 through a pipeline, and the water seal device 11 is connected with at least one gas auxiliary heating device 7 of the wood vinegar distillation system 1 through a pipeline; the bottom valve 92 of the sealed static separation device is connected with at least one distillation furnace 5 of the wood vinegar distillation system 1 through a pipeline; the sealed stationary separation device side valve 91 is connected with the stationary separation device 10 through a pipeline; a vacuum pump 14 is arranged on a pipeline between the water sealing device 11 and the sealing standing separation device 9; a distillation furnace pressure control valve 52 is arranged on a pipeline at the top of the distillation furnace 5; the top of the stationary separation apparatus 10 is provided with an opening 103.

A vacuum pump 14 is arranged on a pipeline between the water sealing device 11 and the sealing standing separation device 9; the wood vinegar separating system 2 further comprises a wood tar storage device 12 and a wood vinegar storage device 13, and a bottom valve 102 of the standing separating device is connected with the wood tar storage device 12 through a pipeline; the stationary separation device side valve 101 is connected to the pyroligneous liquor storage device 13 through a pipe.

The process for producing pyroligneous liquor by adopting the system comprises the following steps of:

step 1: placing the wood raw materials into a smashing device 4 for smashing, starting a heating device 6, and placing the smashed wood raw materials into a distillation furnace 5; the wood raw material is apple branches.

Step 2: the distilled fraction is divided into three stages, namely a first stage distillation, a second stage distillation and a third stage distillation

First stage distillation

The distillation temperature is controlled at 120 ℃, the distillation time is 3h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

Second stage distillation

The distillation temperature is controlled at 265 ℃, the distillation time is 2 hours, when the pressure in the distillation furnace is 2.0 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for burning, and the vacuum degree is controlled at 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 3200 ℃, the distillation time is 5 hours, when the pressure in the distillation furnace is 1.5 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water sealing device 11 and is led into the gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

All the liquid is placed in the device of the static separation device 10 for 10 hours, the unstable pyroligneous liquor component on the upper layer in the static separation device 10 is removed, the liquid at the bottom is discharged from the bottom valve 102 of the static separation device, and then the solution discharged from the side valve 101 of the static separation device is pyroligneous liquor.

Example 2. As shown in fig. 5, this embodiment is different from embodiment 1 in that: the side wall of the static separation device 10 is provided with a liquid outlet hole 106; the side valve 101 of the static separation device comprises a floating plate valve 107 capable of sealing a liquid outlet hole 106 on the side wall of the static separation device, a floating plate valve supporting spring 108 and a floating plate valve horizontal limiting vertical plate 109 arranged on the bottom surface of the static separation device 10, when the liquid in the static separation device is smaller than or equal to a certain density, the floating plate valve 107 descends under the action of buoyancy and self gravity and seals the liquid outlet hole 106 on the side wall of the static separation device, when the liquid in the static separation device 10 is larger than a certain density, the floating plate valve 107 floats upwards under the action of the buoyancy and the floating plate valve supporting spring 108 and does not seal the liquid outlet hole 106 on the side wall of the static separation device any more, the floating plate valve 107 is positioned between the side wall of the static separation device where the liquid outlet hole 106 is positioned and the floating plate valve horizontal limiting vertical plate 109, the floating plate valve 107 contacts the side wall where the liquid outlet hole 106 is positioned, and the plate valve horizontal limiting vertical plate 109, and a plurality of through holes 105 are horizontally arranged on the floating plate valve 107. The length of the floating plate valve 107 is at least 1.5 times larger than the diameter of the outlet aperture 106. The height of the top surface of the floating plate valve horizontal limiting vertical plate 109 is larger than the height of the top surface of the liquid outlet hole 106.

The bottom surface of the static separation device 10 is provided with a bottom liquid outlet hole 1010, the bottom valve 102 of the static separation device comprises a floating valve 1011 arranged on the bottom liquid outlet hole 1010 of the bottom surface of the static separation device, the bottom surface of the floating valve 1011 is provided with a plunger 1012 inserted into the bottom liquid outlet hole 1010 of the bottom surface of the static separation device, and the diameter of the plunger 1012 is slightly smaller than the diameter of the bottom liquid outlet hole 1010 of the bottom surface of the static separation device; when the liquid at the bottom of the stationary separation device 10 is greater than a certain density, under the action of the buoyancy, the floating valve 1011 is separated from the bottom liquid outlet 1010, and when the liquid at the bottom of the stationary separation device 10 is less than a certain density, under the neutral action, the floating valve 1011 is in contact with the bottom liquid outlet 1010, thereby preventing the liquid at the bottom of the stationary separation device 10 from flowing out from the bottom liquid outlet.

The wood vinegar separating system 2 further comprises an activated carbon adsorption device 131, and the valve 101 at the side of the standing separation device is connected with the activated carbon adsorption device 131 through a pipeline.

Example 3. As shown in fig. 2, this embodiment is different from embodiment 1 in that: there are two wood vinegar distillation systems 1. The water sealing device 11 is connected with the gas auxiliary heating devices 7 of the two wood vinegar distillation systems 1 through pipelines.

Comprises the following steps:

step 1: placing the wood raw materials into a smashing device 4 for smashing, starting a heating device 6, and placing the smashed wood raw materials into a distillation furnace 5; the wood raw material is pear tree branches.

First stage distillation

The distillation temperature is controlled at 135 ℃ and the distillation time is 3h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline to burn, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

second stage distillation

The distillation temperature is controlled at 280 ℃, the distillation time is 3 hours, when the pressure in the distillation furnace is 2.0 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

Third stage distillation

The distillation temperature is controlled at 350 ℃, the distillation time is 5 hours, when the pressure in the distillation furnace is 2.5 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

step 3: separation

Standing all the liquid in a device of a standing separation device 10 for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom from a bottom valve 102 of the standing separation device, discharging the solution from a side valve 101 of the standing separation device, and placing the solution into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the activated carbon used is 3% of the mass of the crude wood vinegar.

Example 4. As shown in fig. 3, this embodiment is different from embodiment 3 in that: the wood vinegar separating system 2 comprises a negative pressure sealing and standing separating device 15, wherein the negative pressure sealing and standing separating device 15 is arranged on a pipeline between a sealing and standing separating device side valve 91 and the standing separating device 10; the side wall of the negative pressure sealing and standing separation device 15 is provided with a negative pressure sealing and standing separation device side valve 151, and the bottom of the negative pressure sealing and standing separation device 15 is provided with a negative pressure sealing and standing separation device bottom valve 152; the negative pressure sealing static separation device side valve 151 is connected with the static separation device 10 through a pipeline, and the negative pressure sealing static separation device bottom valve 152 is communicated with a pipeline between the sealing static separation device bottom valve 92 and the distillation furnace 5 through a pipeline; the top of the negative pressure sealing static separation device 15 is connected with a low-pressure water seal device 17 through a pipeline, and the low-pressure water seal device 17 is connected with a pipeline between the water seal device 11 and the gas auxiliary heating device 7 through a pipeline; a vacuum pump 16 of the negative pressure sealing static separation device is arranged on a pipeline between the low pressure water seal device 17 and the negative pressure sealing static separation device 15.

the method is characterized by comprising the following steps of:

step 1: placing the wood raw materials into a smashing device 4 for smashing, starting a heating device 6, and placing the smashed wood raw materials into a distillation furnace 5; the wood raw material is jujube tree branches.

First stage distillation

The distillation temperature is controlled at 135 ℃ and the distillation time is 3h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline to burn, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the negative pressure sealed static separation device 15;

second stage distillation

The distillation temperature is controlled at 265 ℃, the distillation time is 3 hours, when the pressure in the distillation furnace is 1.6 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the negative pressure sealed static separation device 15;

Third stage distillation

The distillation temperature is controlled at 295 ℃, the distillation time is 3.2h, when the pressure in the distillation furnace is 1.8 atm, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water sealing device 11 and is led into the gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

step 3: separation

A step of performing low-pressure stationary separation in a vacuum seal stationary separation device 15 for a stationary time of 1h; when the pressure in the negative pressure sealing and standing separation device 15 is 1.5 atmospheres, a vacuum pump 16 of the negative pressure sealing and standing separation device is started, flue gas in the negative pressure sealing and standing separation device 15 is led into a low-pressure water seal device 17 and is led into a fuel gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the low-pressure static separation is finished, introducing liquid at the bottom of the negative pressure sealing static separation device 15 into the distillation furnace 5, and introducing the rest liquid in the negative pressure sealing static separation device 15 into the static separation device 10;

Standing all the liquid in a device of a standing separation device 10 for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom from a bottom valve 102 of the standing separation device, discharging the solution from a side valve 101 of the standing separation device, and placing the solution into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar.

Example 5. As shown in fig. 4, this embodiment is different from embodiment 4 in that: the distillation furnace 5 is provided with a charcoal discharge hole 51, the wood vinegar separating system 2 also comprises a steam activating device 132, and the steam activating device 132 comprises a heating device; the water seal device 11 is connected with a heating device of the water vapor activation device 132 through a pipeline.

The refining process comprises the following steps:

step 1: placing the wood raw materials into a smashing device 4 for smashing, starting a heating device 6, and placing the smashed wood raw materials into a distillation furnace 5; the wood raw material is branches of apricot trees.

First stage distillation

The distillation temperature is controlled at 95-135 ℃ and the distillation time is 1-3h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

Second stage distillation

The distillation temperature is controlled at 160 ℃, the distillation time is 3 hours, when the pressure in the distillation furnace is 1.6 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 340 ℃, the distillation time is 3.5h, when the pressure in the distillation furnace is 2.4 atm, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water sealing device 11 and is led into the gas auxiliary heating device 7 through the pipeline for burning, and the vacuum degree is controlled at 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

Standing all the liquid in the device of the standing separation device 10 for 10 hours, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom of the standing separation device from a bottom valve 102 of the standing separation device, and then placing the solution discharged from a side valve 101 of the standing separation device into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the activated carbon is 5% of the mass of the crude wood vinegar. The preparation method of the activated carbon comprises the following steps: after charcoal is taken out from the charcoal outlet 51 of the distillation furnace 5, the charcoal is put into the steam activation device 132, and the gas of the heating device of the steam activation device 132 comes from the water seal device 11.

Example 6. The present embodiment is different from embodiment 1 in that the process for producing pyroligneous liquor comprises the steps of:

First stage distillation

Second stage distillation

The distillation temperature is controlled at 240 ℃, the distillation time is 3h, when the pressure in the distillation furnace is 2.0 atm, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for burning, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 300 ℃, the distillation time is 5 hours, when the pressure in the distillation furnace is 1.5 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

Example 7. The present embodiment differs from embodiment 3 in that the production process includes the following steps:

First stage distillation

The distillation temperature is controlled at 130 ℃, the distillation time is 3h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

Second stage distillation

The distillation temperature is controlled at 220 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.8 atm, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water sealing device 11 and is led into the gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 345 ℃, the distillation time is 5 hours, when the pressure in the distillation furnace is 2 atmospheres, the distillation furnace pressure control valve 52 is opened, flue gas in the distillation furnace is led into the condenser 8, liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

Standing all the liquid in the device of the standing separation device 10 for 10 hours, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom of the standing separation device from a bottom valve 102 of the standing separation device, and then placing the solution discharged from a side valve 101 of the standing separation device into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar.

Example 8. The present embodiment differs from embodiment 4 in that the production process includes the following steps:

First stage distillation

The distillation temperature is controlled at 120 ℃, the distillation time is 1h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the negative pressure sealed static separation device 15;

Second stage distillation

The distillation temperature is controlled at 150 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.5-2.0 atm, the pressure control valve 52 of the distillation furnace is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 for burning through a pipeline, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the negative pressure sealed static separation device 15;

third stage distillation

The distillation temperature is controlled at 350 ℃, the distillation time is 3-5h, when the pressure in the distillation furnace is 1.5-2.5 atm, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 for burning through a pipeline, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

standing all the liquid in the device of the standing separation device 10 for 8 hours, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom from a bottom valve 102 of the standing separation device, discharging the solution from a side valve 101 of the standing separation device, and placing the solution into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the activated carbon used is 4% of the mass of the crude wood vinegar.

Example 9. The present embodiment differs from embodiment 4 in that the production process includes the following steps:

First stage distillation

second stage distillation

The distillation temperature is controlled at 280 ℃, the distillation time is 2 hours, when the pressure in the distillation furnace is 2.0 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the negative pressure sealed static separation device 15;

Third stage distillation

The distillation temperature is controlled at 350 ℃, the distillation time is 3 hours, when the pressure in the distillation furnace is 2.5 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

step 3: separation

A step of performing low-pressure static separation in a negative pressure sealed static separation device 15, wherein the static time is 1-2h; when the pressure in the negative pressure sealing and standing separation device 15 is 1.2 atmospheres, a vacuum pump 16 of the negative pressure sealing and standing separation device is started, flue gas in the negative pressure sealing and standing separation device 15 is led into a low-pressure water seal device 17 and is led into a fuel gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the low-pressure static separation is finished, introducing liquid at the bottom of the negative pressure sealing static separation device 15 into the distillation furnace 5, and introducing the rest liquid in the negative pressure sealing static separation device 15 into the static separation device 10;

Example 10. The present embodiment differs from embodiment 5 in that the refining process includes the following steps:

First stage distillation

The distillation temperature is controlled at 95 ℃ and the distillation time is 1h, flue gas in a distillation furnace is led into a condenser 8, liquid formed after the flue gas is condensed is led into a sealed static separation device 9, a vacuum pump 14 is started, gas volatilized from the liquid in the sealed static separation device 9 is led into a water seal device 11 and is led into a gas auxiliary heating device 7 through a pipeline to burn, and the vacuum degree is controlled at 0.085-0.09Mpa; after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

Second stage distillation

The distillation temperature is controlled at 150 ℃, the distillation time is 2 hours, when the pressure in the distillation furnace is 2 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed by condensing the flue gas is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 300 ℃, the distillation time is 4 hours, when the pressure in the distillation furnace is 2 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed by condensing the flue gas is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for burning, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

Standing all the liquid in the device of the standing separation device 10 for 9 hours, removing unstable pyroligneous liquor components on the upper layer in the standing separation device 10, discharging the liquid at the bottom from a bottom valve 102 of the standing separation device, discharging the solution from a side valve 101 of the standing separation device, and placing the solution into an activated carbon adsorption device 131 for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar. The preparation method of the activated carbon comprises the following steps: after charcoal is taken out from the charcoal outlet 51 of the distillation furnace 5, the charcoal is put into the steam activation device 132, and the gas of the heating device of the steam activation device 132 comes from the water seal device 11.

Example 11. The present embodiment differs from embodiment 5 in that the refining process includes the following steps:

First stage distillation

Second stage distillation

The distillation temperature is controlled at 200 ℃, the distillation time is 3 hours, when the pressure in the distillation furnace is 2.0 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water seal device 11 and is led into the gas auxiliary heating device 7 through the pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device 9 into the distillation furnace 5, and introducing the rest liquid in the sealed static separation device 9 into the static separation device 10;

third stage distillation

The distillation temperature is controlled at 320 ℃, the distillation time is 5 hours, when the pressure in the distillation furnace is 2.5 atmospheres, the distillation furnace pressure control valve 52 is opened, the flue gas in the distillation furnace is led into the condenser 8, the liquid formed after the flue gas is condensed is led into the sealed static separation device 9, the vacuum pump 14 is started, the gas volatilized from the liquid in the sealed static separation device 9 is led into the water sealing device 11 and is led into the gas auxiliary heating device 7 through a pipeline for combustion, and the vacuum degree is controlled to be 0.085-0.09Mpa; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device 9 into a distillation furnace 5;

Step 3: separation

The charcoal produced in the above example is tested, and the charcoal prepared by the method has high yield which reaches more than 27-29%; ash content of charcoal is lower than 9.92%; the volatile content is lower than 11.05%; the fixed carbon content is higher than 83%; the specific surface area of charcoal is large and reaches 195-249m2/g; the heat value of the charcoal is high, the heat value of each gram of charcoal reaches over 32000J, and the heat value of the charcoal reaches the standard of high-quality charcoal products. The wood vinegar produced in the above example has a moisture content of 89.9-90.5% as measured by Karl Fisher method. After the sample is extracted and concentrated by diethyl ether, the organic components in the sample are identified and the relative content of the organic components is measured by adopting gas chromatography-mass spectrometry on-line technology analysis. The experiment result shows that the wood vinegar liquid contains acetic acid as main component, acetic acid in 50.3-51.2 wt% and 18 kinds of 45-62 kinds of alcohol, ester, ketone, phenol, etc. The color of the wood vinegar produced by the invention is light yellow brown or light red brown in examples 1-9, the liquid produced by examples 10 and 11 is light brown, the natural wood vinegar contains more than 200 components, 45-52 components of the wood vinegar produced by the invention indicate that some components which are easy to oxidize and change are separated. The small amount of wood vinegar dipped in each embodiment is dripped on white paper, and after the wood vinegar is dried, the wood vinegar is observed to be light brown transparent liquid, and no black or black brown liquid stain appears on one side, which indicates that the wood vinegar is relatively stable and is not easy to be oxidized by oxygen in the air or generate photochemical reaction. And placing the produced pyroligneous liquor into a test tube for standing for 5 minutes, wherein suspended matters are not generated, which indicates that the pyroligneous liquor has good quality.

The above-mentioned embodiments are only for understanding the present invention, and are not intended to limit the technical solutions described in the present invention, and a person skilled in the relevant art may make various changes or modifications based on the technical solutions described in the claims, and all equivalent changes or modifications are intended to be included in the scope of the claims of the present invention. The present invention is not described in detail in the present application, and is well known to those skilled in the art.

Claims

1. A refining system for refining wood vinegar by using wood raw materials, comprising: a feeding system (3), a plurality of wood vinegar distillation systems (1) and a wood vinegar separation system (2);

the feeding system (3) comprises a crushing device (4);

the wood vinegar distillation system (1) comprises a distillation furnace (5), a heating device (6) and a gas auxiliary heating device (7);

the wood vinegar separating system (2) comprises a condenser (8), a sealing standing separating device (9), a standing separating device (10) and a water sealing device (11); a side valve (91) of the sealing and standing separation device is arranged on the side wall of the sealing and standing separation device (9), and a bottom valve (92) of the sealing and standing separation device is arranged at the bottom of the sealing and standing separation device (9); a side wall of the static separation device (10) is provided with a static separation device side valve (101), and the bottom of the static separation device (10) is provided with a static separation device bottom valve (102); the top of the distillation furnace (5) is connected with a condenser (8) through a pipeline, and the condenser (8) is connected with a sealed static separation device (9) through a pipeline; the top of the sealed static separation device (9) is connected with a water seal device (11) through a pipeline, and the water seal device (11) is connected with a gas auxiliary heating device (7) of at least one wood vinegar distillation system (1) through a pipeline; the bottom valve (92) of the sealed static separation device is connected with the distillation furnace (5) of at least one wood vinegar distillation system (1) through a pipeline; the valve (91) at the side of the sealed static separation device is connected with the static separation device (10) through a pipeline; a vacuum pump (14) is arranged on a pipeline between the water sealing device (11) and the sealing and standing separation device (9); a distillation furnace pressure control valve (52) is arranged on a pipeline at the top of the distillation furnace (5); an opening (103) is arranged at the top of the static separation device (10);

A liquid outlet hole (106) is arranged on the side wall of the static separation device (10); the side valve (101) of the static separation device comprises a floating plate valve (107) and a floating plate valve supporting spring (108), wherein the floating plate valve supporting spring can seal a liquid outlet hole (106) on the side wall of the static separation device, the floating plate valve horizontal limiting vertical plate (109) is arranged on the bottom surface of the static separation device (10), when the liquid in the static separation device is smaller than or equal to a certain density, the floating plate valve (107) descends under the action of buoyancy and self gravity and seals the liquid outlet hole (106) on the side wall of the static separation device, when the liquid in the static separation device (10) is larger than the certain density, the floating plate valve (107) floats upwards under the action of the buoyancy and the floating plate valve supporting spring (108) and does not seal the liquid outlet hole (106) on the side wall of the static separation device, the floating plate valve (107) is positioned between the side wall of the static separation device where the liquid outlet hole (106) is positioned and the floating plate valve horizontal limiting vertical plate (109), the floating plate valve (107) is in contact with the side wall where the liquid outlet hole (106) is positioned, and the floating plate valve horizontal limiting vertical plate (109) is horizontally provided with a plurality of through holes (105);

a bottom liquid outlet hole (1010) is formed in the bottom surface of the static separation device (10), the bottom valve (102) of the static separation device comprises a floating valve (1011) arranged on the bottom liquid outlet hole (1010) in the bottom surface of the static separation device, a plug rod (1012) inserted into the bottom liquid outlet hole (1010) in the bottom surface of the static separation device is arranged on the bottom surface of the floating valve (1011), and the diameter of the plug rod (1012) is slightly smaller than that of the bottom liquid outlet hole (1010) in the bottom surface of the static separation device; when the liquid at the bottom of the static separation device (10) is greater than a certain density, under the action of buoyancy, the floating valve (1011) is separated from the bottom liquid outlet hole (1010), the liquid at the bottom of the static separation device (10) flows out from the bottom liquid outlet hole, and when the liquid at the bottom of the static separation device (10) is less than a certain density, under the neutral action, the floating valve (1011) is contacted with the bottom liquid outlet hole (1010), so that the liquid at the bottom of the static separation device (10) is prevented from flowing out from the bottom liquid outlet hole.

2. A refining system for refining pyroligneous liquor from wood raw materials as claimed in claim 1, wherein: the number of the wood vinegar distillation systems (1) is 1-6; the wood vinegar separating system (2) further comprises a wood tar storage device (12) and a wood vinegar storage device (13), and a bottom valve (102) of the standing separating device is connected with the wood tar storage device (12) through a pipeline; the valve (101) at the side of the standing separation device is connected with the pyroligneous liquor storage device (13) through a pipeline.

3. A refining system for refining pyroligneous liquor using wood raw materials as claimed in any one of claims 1 to 2, wherein: the wood vinegar separating system (2) comprises a negative pressure sealing and standing separating device (15), wherein the negative pressure sealing and standing separating device (15) is arranged on a pipeline between a sealing and standing separating device side valve (91) and a standing separating device (10); a side valve (151) of the negative pressure sealing and standing separation device is arranged on the side wall of the negative pressure sealing and standing separation device (15), and a bottom valve (152) of the negative pressure sealing and standing separation device is arranged at the bottom of the negative pressure sealing and standing separation device (15); the negative pressure sealing static separation device side valve (151) is connected with the static separation device (10) through a pipeline, and the negative pressure sealing static separation device bottom valve (152) is communicated with a pipeline between the sealing static separation device bottom valve (92) and the distillation furnace (5) through a pipeline; the top of the negative pressure sealing static separation device (15) is connected with a low pressure water seal device (17) through a pipeline, and the low pressure water seal device (17) is connected with a pipeline between the water seal device (11) and the fuel gas auxiliary heating device (7) through a pipeline; a vacuum pump (16) of the negative pressure sealing static separation device is arranged on a pipeline between the low pressure water sealing device (17) and the negative pressure sealing static separation device (15).

4. A refining system for refining pyroligneous liquor using wood raw materials as claimed in any one of claims 1 to 2, wherein: the wood vinegar separating system (2) further comprises an active carbon adsorption device (131), and the valve (101) at the side of the standing separation device is connected with the active carbon adsorption device (131) through a pipeline.

5. A refining system for refining pyroligneous liquor using wood raw materials as claimed in any one of claims 1 to 2, wherein: the distillation furnace (5) is provided with a charcoal discharge hole (51), the wood vinegar separating system (2) also comprises a steam activating device (132), and the steam activating device (132) comprises a heating device; the water sealing device (11) is connected with a heating device of the water vapor activation device (132) through a pipeline.

6. A process for refining pyroligneous liquor using a refining system according to any of claims 1 to 2, characterized by the steps of:

step 1: crushing wood raw materials in a crushing device (4), starting a heating device (6), and putting the crushed wood raw materials in a distillation furnace (5);

step 2: the distilled fraction is divided into three stages, namely first stage distillation, second stage distillation and third stage distillation

The distillation temperature is controlled at 95-135 ℃ and the distillation time is 1-3h, flue gas in a distillation furnace is led into a condenser (8), liquid formed after the flue gas is condensed is led into a sealed static separation device (9), a vacuum pump (14) is started, gas volatilized from the liquid in the sealed static separation device (9) is led into a water seal device (11) and is led into a gas auxiliary heating device (7) through a pipeline for combustion;

after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device (9) into a distillation furnace (5), and introducing the rest liquid in the sealed static separation device (9) into a static separation device (10);

second stage distillation

The distillation temperature is controlled at 136-280 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.5-2.0 atm, a distillation furnace pressure control valve (52) is opened, flue gas in the distillation furnace is led into a condenser (8), liquid formed after the flue gas is condensed is led into a sealed static separation device (9), a vacuum pump (14) is opened, and gas volatilized from the liquid in the sealed static separation device (9) is led into a water sealing device (11) and is led into a gas auxiliary heating device (7) for combustion through a pipeline; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device (9) into a distillation furnace (5), and introducing the rest liquid in the sealed static separation device (9) into a static separation device (10);

Third stage distillation

The distillation temperature is controlled to 281-350 ℃, the distillation time is 3-5h, when the pressure in the distillation furnace is 1.5-2.5 atm, a distillation furnace pressure control valve (52) is opened, flue gas in the distillation furnace is led into a condenser (8), liquid formed after the flue gas is condensed is led into a sealed static separation device (9), a vacuum pump (14) is opened, and gas volatilized from the liquid in the sealed static separation device (9) is led into a water sealing device (11) and is led into a gas auxiliary heating device (7) for combustion through a pipeline; after the third-stage distillation is finished, introducing all liquid in the sealed static separation device (9) into a distillation furnace (5);

step 3: separation

And (3) standing all the liquid in the standing separation device (10) for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device (10), discharging the liquid at the bottom from a bottom valve (102) of the standing separation device, and then discharging the solution from a side valve (101) of the standing separation device to obtain the pyroligneous liquor.

7. A process for refining pyroligneous liquor using a refining system according to claim 3, characterized by the steps of:

the method is characterized by comprising the following steps of:

after the distillation of the first stage is finished, introducing the liquid at the bottom in the sealed static separation device (9) into a distillation furnace (5), and introducing the rest liquid in the sealed static separation device (9) into a negative pressure sealed static separation device (15);

second stage distillation

The distillation temperature is controlled at 136-280 ℃, the distillation time is 2-3h, when the pressure in the distillation furnace is 1.5-2.0 atm, a distillation furnace pressure control valve (52) is opened, flue gas in the distillation furnace is led into a condenser (8), liquid formed after the flue gas is condensed is led into a sealed static separation device (9), a vacuum pump (14) is opened, and gas volatilized from the liquid in the sealed static separation device (9) is led into a water sealing device (11) and is led into a gas auxiliary heating device (7) for combustion through a pipeline; after the second-stage distillation is finished, introducing the liquid at the bottom in the sealed static separation device (9) into a distillation furnace (5), and introducing the rest liquid in the sealed static separation device (9) into a negative pressure sealed static separation device (15);

Third stage distillation

step 3: separation

A step of low-pressure static separation in a negative-pressure sealed static separation device (15), wherein the static time is 1-2h; when the pressure in the negative pressure sealing static separation device (15) is 1.2-1.5 atmospheres, a vacuum pump (16) of the negative pressure sealing static separation device is started, and flue gas in the negative pressure sealing static separation device (15) is led into a low-pressure water seal device (17) and is led into a fuel gas auxiliary heating device (7) through a pipeline for combustion; after the low-pressure static separation is finished, introducing liquid at the bottom of the negative-pressure sealed static separation device (15) into a distillation furnace (5), and introducing the rest liquid in the negative-pressure sealed static separation device (15) into a static separation device (10);

8. A process for refining pyroligneous liquor using a refining system according to claim 4, comprising the steps of:

Second stage distillation

third stage distillation

Step 3: separation

Standing all the liquid in a standing separation device (10) for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device (10), discharging the liquid at the bottom from a bottom valve (102) of the standing separation device, discharging the solution from a side valve (101) of the standing separation device, and placing the solution into an activated carbon adsorption device (131) for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar.

9. A process for refining pyroligneous liquor using a refining system according to claim 5, comprising the steps of:

second stage distillation

third stage distillation

Step 3: separation

Standing all the liquid in a standing separation device (10) for 8-10h, removing unstable pyroligneous liquor components on the upper layer in the standing separation device (10), discharging the liquid at the bottom from a bottom valve (102) of the standing separation device, discharging the solution from a side valve (101) of the standing separation device, and placing the solution into an activated carbon adsorption device (131) for adsorption, wherein the adsorbed liquid is pyroligneous liquor; the mass of the active carbon is 3-5% of the mass of the crude wood vinegar; the preparation method of the activated carbon comprises the steps of taking out charcoal from a charcoal discharge hole (51) of a distillation furnace (5), and then putting the charcoal into a water vapor activation device (132), wherein fuel gas of a heating device of the water vapor activation device (132) is from a water seal device (11).