CN103420956A - Furfural refining technology - Google Patents

Abstract

A furfural refining technology relates to the technical field of chemical engineering, and comprises the following steps: firstly, opening a water ring vacuum pump, and pumping about 1000 kg furfural with the concentration of 99.0% into a reaction kettle; opening a rectifying kettle steam inlet valve, starting to heat, sampling and detecting the discharging content of furfural when the liquid level of a light composition tank reaches 10 cm, switching a discharging valve to a B tank and closing an A tank feeding valve when the furfural content is greater than 99.5%; when the liquid level of the rectifying kettle is about 100 L, stopping rectification, closing steam heating, and preparing to discharge materials; after a test shows that the obtained materials are qualified, discharging, barreling, and pasting product labels and certifications, wherein the net weight of each barrel is 240 kg as per the packaging requirement; further, packaging furfural of the A tank with steel barrels, and labeling for the follow-up treatment. According to the invention, the preparing technology is simple, the operation is convenient, the material heat is fully utilized, the energy consumption is reduced, and the generated pollutants are reduced.

Description

A kind of furfural treatment technique

Technical field

The present invention relates to chemical technology field, be specifically related to a kind of furfural treatment technique.

Background technology

Furfural formal name used at school furtural, it is a kind of important industrial chemicals, industrial purposes widely arranged, can be as the selective solvent of unsaturated fatty acids compounds of group in the separating saturated fatty compounds of group, be also the raw material of producing various furfuran compounds, its derived product covers all conglomeraties such as petrochemical complex, synthetic resins, food, medicine and synthon.It is through hydrolysis, to be made in acidic solution by straws such as corn cob, bagasse, in production process, in the hydrolyzer bottom, passes into saturation steam, obtains the aldehyde vapour containing furfural 4% ~ 10%, also produces the by products such as acetic acid, methyl alcohol and acetone simultaneously.

Multiple furfural continuous treating flow process is arranged in the world, and complete flow process should comprise three basic craft course: the concentrate of the contained furfural of stoste and preliminary purification; Lower-boiling impurity remove and reclaim furfural; High-boiling-point impurity remove and reclaim furfural.These three processes are mainly realized by water distilling apparatus such as primary tower (comprising compound primary tower), lightness-removing column, dehydration tower and treating towers.But many flow processs are not also fully taken the integrity of above-mentioned technique into account, and the rectification flow of furfural, also at development, by initial simple distillation, batch fractionating, develops into three tower continuous rectifications, four tower continuous rectifications so that five tower continuous rectification flow processs.The main device of five tower process for refining is connected and composed successively by primary tower, lightness-removing column, water wash column, dehydration tower and treating tower, fore-running overhead extraction aldehyde water azeotrope wherein, water wash column is removed the organic acid contained in furfural, saved in the past and to have added in alkali and operation before advancing dehydration tower, and avoided in the furfural product containing except sordid sodium-acetate, lightness-removing column is born low-boiling-point substance extraction task, and high-boiling-point impurity is by the treating tower extraction.By after the condensation of furfural vapour, entering primary tower, do not take full advantage of heat energy in five tower continuous rectifications; And this technique is first to take off gently and wash, lightness-removing column substrate material need to return to primary tower and evaporate; The furfural that simultaneously at the bottom for the treatment of tower, in aldehyde mud, contains 10% left and right, do not processed in five tower continuous rectification techniques again, if directly as fuel, not only wasted the part furfural and also meeting has been polluted to surrounding enviroment.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of preparation method simple, pollution-free, the furfural treatment technique that cost is low.

Technical problem to be solved by this invention realizes by the following technical solutions:

A kind of furfural treatment technique is characterized in that: described process for refining comprises following processing step,

1. feed intake

1. the ring vacuum pump of fetching boiling water, during be less than-0.07mpa of system vacuum degree, start in the about 1000kg suction of 99.0% furfural reactor;

2. rectifying

1. open rectifying still steam inlet valve, start to heat, the initial stage vapor pressure of heating is the 0.3mpa left and right, when the still temperature reaches more than 80 ℃, turns vapor pressure down to 0.05-0.1mpa;

2. note to observe the rectifying condenser outlet, when outlet has distillate to flow out, start to record the initial boiling point temperature, record rectifying still temperature, rectifying tower tower top temperature, vacuum tightness, discharging liquid level later per half an hour;

3. when light constituent tank liquid level reaches 10cm, sampling detects furfural discharging content, and when furfural content is greater than 99.5%, the switching bleeder valve, to the B tank, cuts out A tank feed valve;

4. when the about 100L of rectifying still liquid level residue furfural, switching B tank, to the A tank, stops heating, again extracts 700kg 99.0% furfural to rectifying still;

5. repeat 2., operation 3.;

6. when the about 100L of liquid level of rectifying still, stop rectifying, the steam off heating, prepare discharging;

3. discharging

1. close A tank, B tank feed valve, vacuum extraction valve, connect the nitrogen air inlet, regulate nitrogen reducing valve pressure and be not more than 0.15mpa, give A tank, B tank vacuum breaker;

2. when A tank, B pressure tank meter reading approach 0, prepare discharging;

3. sample examination, require B tank furfural content to be not less than 99.5%;

4. chemically examine qualified after, discharging, barrelling, every barrel of net weight 240kg of packing instructions, stick Product labelling, conformity certification after barrelling;

5. A tank furfural is packed with Tie Tong in addition, and labelled, waits until aftertreatment.

The invention has the beneficial effects as follows: preparation technology of the present invention is simple, and convenient operation takes full advantage of material heat, has reduced energy consumption, has reduced the generation of pollutent.

Embodiment

For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.

Embodiment,

The preparation that driving is front, at first the resistance to air loss of checked operation system, as found leakage point, safeguard in time, production can feed intake while reaching system without obvious the leakage; Check the reactor lubricant level, when not enough, need add lubricating oil; Water in the water ring vacuum pump water tank is added to fixedly liquid level;

1. feed intake

1. the ring vacuum pump of fetching boiling water, during be less than-0.07mpa of system vacuum degree, start in the about 1000kg suction of 99.0% furfural reactor;

2. rectifying

1. open rectifying still steam inlet valve, start to heat, the initial stage vapor pressure of heating is the 0.3mpa left and right, when the still temperature reaches more than 80 ℃, turns vapor pressure down to 0.05-0.1mpa;

2. note to observe the rectifying condenser outlet, when outlet has distillate to flow out, start to record the initial boiling point temperature, record rectifying still temperature, rectifying tower tower top temperature, vacuum tightness, discharging liquid level later per half an hour;

3. when light constituent tank liquid level reaches 10cm, sampling detects furfural discharging content, and when furfural content is greater than 99.5%, the switching bleeder valve, to the B tank, cuts out A tank feed valve;

4. when the about 100L of rectifying still liquid level residue furfural, switching B tank, to the A tank, stops heating, again extracts 700kg 99.0% furfural to rectifying still;

5. repeat 2., operation 3.;

6. when the about 100L of liquid level of rectifying still, stop rectifying, the steam off heating, prepare discharging;

3. discharging

1. close A tank, B tank feed valve, vacuum extraction valve, connect the nitrogen air inlet, regulate nitrogen reducing valve pressure and be not more than 0.15mpa, give A tank, B tank vacuum breaker;

2. when A tank, B pressure tank meter reading approach 0, prepare discharging;

3. sample examination, require B tank furfural content to be not less than 99.5%;

4. chemically examine qualified after, discharging, barrelling, every barrel of net weight 240kg of packing instructions, stick Product labelling, conformity certification after barrelling;

5. A tank furfural is packed with Tie Tong in addition, and labelled, waits until aftertreatment.

The production precaution

1. the resistance to air loss of necessary keeping system, descend as found vacuum tightness, need check in time, and tighten relevant screw and pad.

2. steam heating air pressure can not be too high during rectifying, must be according to the timely steam regulation pressure of discharging speed.

3. airtight package bung immediately after raw material and product use, barrelling, chemical examination.

4. to prevent in production process that material from polluting skin, as occurred, need to rinse with large water gaging in time, send to hospital when serious.

Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (1)

1. a furfural treatment technique, it is characterized in that: described process for refining comprises following processing step,

One. feed intake

1. the ring vacuum pump of fetching boiling water, during be less than-0.07mpa of system vacuum degree, start in the about 1000kg suction of 99.0% furfural reactor;

Two. rectifying

1. open rectifying still steam inlet valve, start to heat, the initial stage vapor pressure of heating is the 0.3mpa left and right, when the still temperature reaches more than 80 ℃, turns vapor pressure down to 0.05-0.1mpa;

2. note to observe the rectifying condenser outlet, when outlet has distillate to flow out, start to record the initial boiling point temperature, record rectifying still temperature, rectifying tower tower top temperature, vacuum tightness, discharging liquid level later per half an hour;

3. when light constituent tank liquid level reaches 10cm, sampling detects furfural discharging content, and when furfural content is greater than 99.5%, the switching bleeder valve, to the B tank, cuts out A tank feed valve;

4. when the about 100L of rectifying still liquid level residue furfural, switching B tank, to the A tank, stops heating, again extracts 700kg 99.0% furfural to rectifying still;

5. repeat 2., operation 3.;

6. when the about 100L of liquid level of rectifying still, stop rectifying, the steam off heating, prepare discharging;

Three. discharging

1. close A tank, B tank feed valve, vacuum extraction valve, connect the nitrogen air inlet, regulate nitrogen reducing valve pressure and be not more than 0.15mpa, give A tank, B tank vacuum breaker;

2. when A tank, B pressure tank meter reading approach 0, prepare discharging;

3. sample examination, require B tank furfural content to be not less than 99.5%;

4. chemically examine qualified after, discharging, barrelling, every barrel of net weight 240kg of packing instructions, stick Product labelling, conformity certification after barrelling;

5. A tank furfural is packed with Tie Tong in addition, and labelled, waits until aftertreatment.