CN1050149C - High-efficiency method for distillation of raw rosin and its apparatus - Google Patents

Abstract

The present invention relates to a new technology for extracting rosin. At present, a preparation method for gum rosin mainly has the problems of high energy consumption, serious pollution of three wastes and insufficient device functions, colors and types of rosin products are poorer than congeneric raw materials in test results, and the disadvantage of crystallization of rosin can not be eradicated. Aiming at the difficult problems which are not solved in a long term, the technology effectively saves energy by about 70%, saves water by about 90% and greatly decreases pollution sources; therefore, the colors and the types of rosin are superior to congeneric raw materials in test results; the disadvantage of crystallization of rosin is overcome by controllable components. The present invention has the essential technology that normal temperature gas is used as a medium, a high temperature and low temperature distillation device is used, a crystallization resistant component of rosin is obtained by a mixed distillation technology, and the problems are solved.

Description

Method for distillation of raw rosin and equipment

The present invention is a kind of ROSIN INDUSTRY High-efficient Production gum rosin and terebinthine method and apparatus. It can allow is engaged in the producer that gum rosin is produced, and in the situation that does not increase raw material and labour, the profit increase at double or several times and produces better social benefit.

At present in ROSIN INDUSTRY, direct fiery working system, owing to be simply equipped, benefit is very poor, shortcoming is too many, eliminating, Let it pass. Steam distillation is produced the method for rosin now, from early fifties till now, has progressively entered the serialization stage, is considered at present technology comparatively progressive in the rosin production. But very unfortunate, in decades, production practices prove, because this technology has some shortcomings that self are difficult to overcome, cause the old factory of some ROSIN INDUSTRY, for these years before the puzzlement not. These shortcomings mainly contain four:

1, energy consumption is large. Steam medium because do spray with water vapour, it is large especially that water vapor need consume " heat energy ".

2, seriously polluted. Because this method is very large with coal, water consumption, so the three wastes " pollution sources " amount is large, the unable burden of producer is administered.

3, the grade look of rosin product number, poorer than the result of same raw material chemical examination. Reason be vapo(u)rizing temperature up to more than 195 ℃, and time of distillation, the shortest also greater than more than 13 minutes, it is still not little therefore to affect the rosin variable color.

4, the evil of CRYSTALLIZATION OF ROSIN can not get radical cure. Because steam distillation to the component of rosin inherence, can't be carried out control. Present technology is namely used vaccum cryogenic distillation, and still not only distillation time is looked and produced and can not accept, and heavy oil is difficult to steam only, and it is qualified that the product softening point can not guarantee; When using high temperature distillation, " levopimaric acid " that plays anti-brilliant effect in the rosin components again all " isomery " do to the greatest extent (at present production generally is to use high temperature distillation), so prior art can't solve rosin from the problem of anti-crystalline substance in essence. Therefore the evil of CRYSTALLIZATION OF ROSIN for these years, as ghost, is reverberated in the ROSIN INDUSTRY midium or long term.

Purpose of the present invention will provide a kind of all deficiencies that can avoid above-mentioned prior art exactly, and can reach the method and apparatus of efficient distillation rosin. Here indication is efficient, not only refers to the energy efficiency height, product quality is high, economic benefit is high and social benefit is high, but also has comprised temperature effect height of the high and distillation of the chronergy of distillation etc.

The present invention efficiently refines fragrant steaming method, it is characterized in that adopting nitrogen or inert gas to make medium, and spray steaming fat liquid makes the separation of vaporizing of turpentine oil in the fat liquid, and allows respectively gas receive to get turpentine oil through condenser in distiller; De-oiling liquid obtains product rosin through packing.

Accompanying drawing is flow chart of the present invention. Wherein Fig. 1 adopts destilling tower to carry out the quantity-produced flow chart; Fig. 2 uses boiler to take the flow process of Batch Process.

Use the main step of method of the present invention to be: (such as accompanying drawing)

1, with the fat liquid to be steamed in the fat liquid storage tank 10, through fine filter 11, behind the flowmeter 13, with preheater 12, fat liquid to be distilled is preheating to 125 ℃～130 ℃.

2, with " closing the vapour coil pipe " in distiller heating distiller, make the temperature in the distiller arrive more than 150 ℃ fast.

3, will have 7 kg/cm with nitrogen or the inert gas of upward pressure, from storage tank 1, put " lively atmosphere jet pipe " ejection of distiller 14 and 16 into by technological requirement, and adjust and close the vapour heating, make the interior temperature stabilization of distiller between 150 ℃～195 ℃, when opening lively atmosphere, start gas transportation machine 2, make the gas in the distiller, by condenser 3 (or 4,5) after the conveyer supercharging, be recovered to again air accumulator 1, constantly circulation.

4, will fat liquid be steamed, through flow score two-way, press process ratio control amount, put into respectively in high temperature 16 (195 ℃) and low temperature 14 (150 ℃) two distillers and distill. Namely can fast release turpentine oil, through mist eliminator 15 at the dielectric gas of operation this moment, run quickly into condenser 3 (oil the time enters 4 in the receipts, enters 5 when receiving heavy oil), by adjusting water, under the effect of condenser, oily vapour or Trace water steam, will liquefy rapidly, separate with inert gas, and flow into salt filter 8, after salt filter dehydration, turpentine oil namely can flow to product oil tank 9, and (oil the time advances 7 in the receipts, advances 6 when receiving heavy oil. Oil and heavy oil need not through 8 dehydrations in the receipts) obtain collecting. And dielectric gas then as mentioned above, on the top of condenser tail, through relevant pipeline, draws back conveyer, after supercharging, sends back to again air accumulator and recycles.

Minute oily means: the high temperature distillation device is mainly by the different temperature of control use, obtain excellent, in, heavy oil; Cryogenic alembic is used atmospheric pressure by watching the Pressure gauge 20 that is contained in behind the lively atmosphere pipe valve to adjust then entirely, reaches minute oily. Its principle is: vapo(u)rizing temperature, distillation time, lively atmosphere consumption, the three is parameter each other. Be time when certain, can achieve the goal with the adjustment vapo(u)rizing temperature; Also can come realize target with the flow of control lively atmosphere. The size of lively atmosphere consumption under certain output, is inversely proportional to the molecular weight of lively atmosphere. The pressure size of lively atmosphere flow, the section with pipeline is inversely proportional to again. So calculate when concrete data need by design, list relevant rules in.

5, after about 8 minutes distillation, heavy oil can steam fat liquid substantially altogether, and the de-oiling thing is that rosin just can at the bottom of two distillers, be put into blending tank 18 simultaneously. Blending tank stirs uses gas, regains behind mist eliminator 15 and heavy oil condenser 5 etc. After high and low temperature rosin mixes, be controlled under the temperature between 130 ℃～140 ℃, enter bucket 24 packings.

6, the coil pipe of holding one's breath of the heating in the distiller is with 360 ℃～380 ℃ superheated vapour " heat supply, the heat release area of coil pipe, guarantee that fat liquid enters distiller after, in one minute, can be warmed up to 150 ℃. This point is to cryogenic alembic, and is particularly important. Because the time of pyrotron distillation here is long, can affect the grade of product; And the time of low-temperature device distillation is long, also can affect the content of " left-handed pine acid ".

Close in the vapour coil pipe steam after the heat release and can mix liquid moisture content is arranged, but the temperature of this indirect steam still has nearly 200 ℃, dewater so collect with vapour tank 17, vapour is then just in time as front workshop section, i.e. use during rosin dissolving.

Dielectric gas generally need not heating system is set in addition, because the specific heat of nitrogen or inert gas is minimum, hear rate is very little, and they generally when the conveyer supercharging power conversion can occur, and enter the gas temperature of air accumulator, generally can be above 160 ℃. If the equipment such as air accumulator are incubated, then temperature also can rise De Genggao, can satisfy the temperature requirement with gas fully.

Requiring preheating as for fat liquid, and make fat liquid be raised to fast 150 ℃ purpose in distiller, all is in order to improve terebinthine vapor partial pressure, for realizing the needs of efficient distillation.

The effect of high temperature distillation device in the present invention, mainly is for by high temperature " isomery ", makes product rosin obtain " abietic acid " component of enough deals; And the effect of cryogenic alembic then is for the anti-crystalline substance " levopimaric acid " of certain deal is arranged in the retained product. The ratio of two kinds of acid is the ratio foundations that determine the charging of high and low temperature distiller. Two kinds of acid content in raw material and in the semi-finished product, and " crystallization trend " in the product rosin etc. will take the concrete analysis data of each factory as foundation, be selected to order into operational procedure by the technologist.

In test, general " levopimaric acid " content is higher, and the crystallization trend of product rosin is less. Make a large amount of " levopimaric acids " of reservation in the product, then vapo(u)rizing temperature also need adopt at 140 ℃ as well. Method and apparatus of the present invention possesses fully but the still condition of flash distillation is arranged in this case.

In order to implement high-efficiency method for distillation of raw rosin of the present invention, reach the crystallization of radical cure rosin, the invention provides a kind of mixing distillation equipment. This equipment comprises the high temperature distillation device, mixes the fragrant tank of storage etc. It is characterized in that it also includes cryogenic alembic; When producing continuously, cryogenic alembic adopts the low temperature distillation tower; During Batch Process, cryogenic alembic adopts the low temperature distillation pot.

The high temperature distillation device is one can make vapo(u)rizing temperature up to 195 ℃ or the equipment of higher final temperature, and its design can be the continuous still tower, also can be the batch distillation pot. The high temperature distillation device is characterized in that: compare with original distillation equipment, heat the coil pipe gross area of remaining silent, all heats of distillation of to guarantee supply; Be in addition the liquid level sky in the distiller, higher than the space of existing equipment, reason is the double negative distillation heat supply of present technique " lively atmosphere ", and gas consumption is large; Especially for cryogenic alembic, because gas speed is very high, even more important.

Cryogenic alembic, its structure and high temperature distillation device are basic identical. And the heating gross area that its feature is just remained silent coil pipe lacks than the high temperature distillation device. Its reason is that the vapo(u)rizing temperature of this equipment is lower, generally can be above 150 ℃.

The high and low temperature distiller can be designed to two monomers (such as attached flow chart), also structure can be designed to be high temperature in one, and be outward the association of low temperature. The device body all is provided with the charging and discharging mouth, with coil pipe heating into and out of steam ports, and visor, thermometer, Pressure gauge etc.; Venthole is with mist eliminator. Be provided with the toroidal nozzle that passes into dielectric gas at the bottom of the distiller, and the dielectric gas import on wall top.

Fat liquid enters before the preheater, and scum silica frost fine filter and flowmeter etc. all are housed on its pipeline separately.

The manufactured materials of equipment: the position that also contacts with finished product and semi-finished product, all use the 1Cr18Ni9Ti steel to make. Gas transportation machine is furnished with air accumulator, and easing valve 2 is housed on the air accumulator, and Pressure gauge 20 etc. On each relevant pipeline, enter for preventing air, with the adverse current of relevant liquid material, check valve all is housed takes precautions against. 25 is overheated steam pipe from boiler in addition, and 26 for leading to the secondary steam pipe of dissolving, and 27 for advancing the fat pipe.

The present invention has the following advantages compared with the prior art:

1, can be a large amount of energy-conservation. Calculate by industrial design, with the vapour method ratio of prior art, economizing on coal to reach more than 70%; Economize on electricity can nearly 70%; Water saving can reach more than 90%.

2, the grade look of product rosin number can surpass with the grade look of raw material chemical examination number. Particularly existing vapour method is produced the materials of one grade or two grades rosin, as use this law production, then most of product all will obtain upgrading. For the product of direct fiery working system, because they all are good raw materials, the rosin of producing but nearly all is off standard. If these raw materials are used this law instead and produced, then product all will be superfine, therefore its profit will be multiplied.

3, minimizing pollution sources that can be a large amount of can make waste residue, waste gas reduce more than 70%; Make waste water reduce more than 90%. Thereby can make the three wastes obtain processing, remission of penalty, and produce social benefit.

4, to the evil of CRYSTALLIZATION OF ROSIN, the condition of effecting a radical cure from has in essence been arranged. To becoming the heavy economic losses of substandard products because of the product crystallization, can be from the disappearance of product crystallization and retrieve. (prior art, the easiest crystallization of fancy produce are thisly reduced to the rosin of off standard by superfine, its price be former superfine valency 70.95%).

5, can reduce labour intensity, improve work situation.

6, can increase income and economize on spending in a large number, reduce cost. Make rosin, turpentine oil product greatly strengthen international competitiveness. And can be to take the new product of this product as the raw material deep processing, also can be with the advantage of high quality and at a reasonable price of raw material, establish oneself in an unassailable position contending for markets. Therefore to the development of ROSIN INDUSTRY, provide beyond doubt more fine prospect.

Use embodiments of the invention, be listed as follows:

Numbering	Working medium	Feeding temperature (℃)	The distillation final temperature (℃)	Distillation time minute	The rosin soft spots (℃)	Rosin grade look number	Same raw material chemical examination look number	Remarks
										1	Helium	130	150	8	76.3	20   1.4	20    2.1	1. same raw material is more than 20 2.2 with the product hierarchy look number statistics of vapour method in the workshop, and is namely poor than the grade look of chemical examination. Namely the rosin grade is 13～23 minutes than the low 2. workshop vapour method distillations of raw material result of laboratory test, and temperature is 195 ℃～225 ℃. 3. the standard-required of rosin softening point is 76 ℃. 4. chemically examine the raw material steam distillation, final temperature is 195 ℃, and distillation time is 17 minutes. 5. the crystallization inspection is to use the acetone method comparison result. 6. other lab work of the sampling of present embodiment is all qualified.
2	Helium	125	180	7	77.2	20   1.7	20    2.1
								3	Nitrogen	130	150	8	76.5	20   1.4	20    2.1
4	Nitrogen	125	180	7	77.4	20   1.7	20    2.1
								5	Helium+nitrogen	130	150	8	76.4	20   1.4	20    2.1
6	Helium+nitrogen	125	180	7	77.3	20   1.6	20    2.1
								7	Neon	130	150	8	76.7	20   1.4	20    2.1
8	Neon	125	180	7	77.5	20   1.6	20    2.1
								9	Nitrogen+neon	130	150	8	77.2	20   1.4	20    2.1
10	Nitrogen+neon	125	180	7	77.8	20   1.6	20    2.1
								11	Argon	130	148	7	77.1	20   1.5	20    2.1
12	Argon	125	180	7	77.9	20   1.7	20    2.1
								13	Nitrogen+argon	130	148	7	76.8	20   1.4	20    2.1
14	Nitrogen+argon	125	180	7	77.5	20   1.7	20    2.1
								15	Xenon	130	145	7	77.3	20   1.5	20    2.1
16	Xenon	125	180	7	77.9	20   1.6	20    2.1
								17	Nitrogen+xenon	130	145	7	76.1	20   1.4	20    2.1
18	Nitrogen+xenon	125	180	7	77.6	20   1.5	20    2.1
								19	Nitrogen+neon+argon	130	145	7	77.4	20   1.4	20    2.1
20	Nitrogen+neon+argon	125	180	7	77.8	20   1.5	20    2.1
								21	Nitrogen neon argon xenon	130	140	7	77.5	20   1.3	20    2.1
22	Nitrogen neon argon xenon	125	180	7	78.2	20   1.4	20    2.1
								23	Helium nitrogen neon argon xenon	130	140	7	77.4	20   1.3	20    2.1
24	Helium nitrogen neon argon xenon	125	180	7	78.1	20   1.4	20    2.1

In above embodiment, the quality index of rosin can both be above standard, and the grade look is number all good than same raw material result of laboratory test; CRYSTALLIZATION OF ROSIN trend, with the sampling that high and low temperature mixes at 1: 1, the result of its chemical examination, the rosin of all producing than vapour method is good.

Claims (5)

1. a distillating method that refines perfume is characterized in that adopting nitrogen or inert gas to make medium, with 195 ℃ or distillation equipment higher and two kinds of functions below 150 ℃, under normal pressure, spray synchronously respectively steaming fat liquid, turpentine oil vaporization in distiller (tower or pot) separately in the fat liquid is separated, and make respectively the vaporization material receive to get turpentine oil through condenser; The steaming excess of two distillers mixes in proportion and obtains product rosin by packing.

2. a kind of method for distillation of raw rosin according to claim 1 is characterized in that the gas that uses is nitrogen, helium, neon, argon, xenon, or its material that mutually mixes.

3. " a kind of method for distillation of raw rosin " according to claim 2 is characterized in that adopting nitrogen or inert gas or its mutual mixture, tells recycling use in the later equipment of condenser or condenser.

4. realize a kind of composition equipment of method for distillation of raw rosin, it is characterized in that it is to increase the circulating running system that is comprised of gas boosting conveying equipment 2 and gas storage equipment 1 at the equipment that original vapour method is produced rosin; And have and to realize that high and low two kinds of final temperatures refine to get distiller (tower or pot) and blending tank 18 equipment of rosin; Refining fragrant final temperature and be 195 ℃ or higher high temperature distillation device 16 and refining fragrant final temperature is cryogenic alembic 14 below 150 ℃, and its internal structure is identical, all has in the device to make the multilayer of fat liquid heating usefulness close the vapour coil pipe, at the bottom of device toroidal nozzle is housed respectively also; The device body all has inlet-outlet connector and the instrument connector of material, gas and heat-carrying agent; Toroidal nozzle is housed in the blending tank; Its concrete connection is as follows:

The contact that is the material turnover is that the supplied materials (fat liquid) in 10 connects by the last fat liquid mouth that goes out of inlet tube 27 and the upper operation (clarification) of rosin production; 10 outlet connects with 11 import, and 11 outlet connects with separately 13 imports respectively, and 13 outlet connects with 12 import separately again separately, and 12 outlet connects with 14,16 import respectively again separately; 14 and 16 outlet then all connects with 18 import; 18 outlet then connects with the packing barrel inlet tube of operation under the rosin production through 23; For turpentine oil, then 3 lower outlet connects with 8 import, and 8 outlet connects with 9 import; 4 lower outlet connects with 7 import again; Same 5 lower outlet connects with 6 import.

5. equipment according to claim 4 is characterized in that the high and low temperature distiller is two monomers or an assembly; Assembly is chuck pot or the chuck tower of two concentric cylindrical shells; Device high-temperature heating coil pipe and jet pipe in the inner core of chuck pot; Device low-temperature heat coil pipe and jet pipe between inner/outer tube; The chuck tower respectively saves the bottom jet pipe of inner barrel device high-temperature heating coil pipe and each section; Each saves the bottom jet pipe that installs low-temperature heat coil pipe and each section between inner/outer tube.

Images