CN102944642B - A kind of preparation method of iodine value reagent of improvement - Google Patents
A kind of preparation method of iodine value reagent of improvement Download PDFInfo
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- CN102944642B CN102944642B CN201210479805.XA CN201210479805A CN102944642B CN 102944642 B CN102944642 B CN 102944642B CN 201210479805 A CN201210479805 A CN 201210479805A CN 102944642 B CN102944642 B CN 102944642B
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- chlorine
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Abstract
The present invention relates to a kind of preparation method of iodine value reagent of improvement, step is: the preparation glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution; By manganese dioxide and concentrated hydrochloric acid preparing chlorine gas, chlorine is through saturated aqueous common salt, after concentrated sulphuric acid drying with Iod R in the glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution after, obtain the glacial acetic acid of lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution; Regulate with the glacial acetic acid of iodine and the glacial acetic acid of methenyl choloride or phenixin or cyclohexane mixed solution and lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution; The reaction residue of preparation of chlorine is through process, and recovery obtains manganese dioxide and recycles.The invention has the advantages that: be unreacted manganese dioxide, manganous chloride in the reaction residue of preparation of chlorine, unreacted hydrochloric acid, obtain manganese dioxide, method environmental protection through process recovery.
Description
Technical field
The present invention relates to a kind of preparation method of iodine value reagent of improvement, relate to a kind of iodine and cl molar ratio specifically and be similar to the glacial acetic acid of the lodine chloride of 1 and methenyl choloride or phenixin or cyclohexane mixed solution.
Background technology
It is special and be topmost addition reaction chemical reagent that iodine value reagent measures the one of the product iodine numbers (degree of unsaturation) such as grease, fatty acid, surfactant.
GB/T 5532-2008, GB/T 9104-2008 and ISO 3961-2009 are the acetic acid solutions with lodine chloride, when the acetic acid solution temperature of lodine chloride is slightly low, easily solidify, and especially winter is more obvious, and practical operation is very inconvenient.With the glacial acetic acid of lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution, the iodine value reagent namely improved (wijs reagent), just can solve the problem that low temperature solidifies.A kind of solvent compound in concrete acetic acid and methenyl choloride or phenixin or cyclohexane prepares mixed solvent, see that material which solubleness in methenyl choloride or phenixin or cyclohexane three kinds of solvents needing to measure iodine number is large, just select large that of solubleness, a kind of blending ratio in solvent acetic acid and methenyl choloride or phenixin or cyclohexane three kinds of solvents is 4:1 ~ 5:1.
National standard is all be added drop-wise to preparing chlorine gas in potassium permanganate with concentrated hydrochloric acid, and invalid patent CN1236101A also proposes " hydrochloric acid drips in potassium permanganate, then allows the chlorine generated first by using after washing, concentrated sulphuric acid drying ".Should could remove hydrogen chloride gas with saturated common salt water washing, and chlorine hardly solvent in saturated aqueous common salt.Practical operation concentrated hydrochloric acid is added drop-wise to preparing chlorine gas in potassium permanganate, find that reaction generates crumby brown material capping, affect the preparation speed of chlorine, and preparation of chlorine bottle is difficult to cleaning, be speculated as crumby manganese dioxide parcel potassium permanganate, the continuation hindering chlorine produces, and affects preparation of chlorine; Be added drop-wise in potassium dichromate with concentrated hydrochloric acid and also can prepare chlorine, but in the raffinate in preparation of chlorine bottle, remaining potassium dichromate is the unfriendly material of environment; Also can produce chlorine with potash chlorate and concentrated hydrochloric acid reaction, and chlorine output ratio is very large, because there is the problems such as subsidiary reaction chlorine dioxide, chlorine is impure, is difficult to purified treatment.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of preparation method of iodine value reagent of easy to operate, environmental protection.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of iodine value reagent of improvement, and its innovative point is: described step is:
(1) glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution is prepared;
(2) chlorine obtained by certain fineness manganese dioxide and concentrated hydrochloric acid, the chlorine of preparation removes hydrogen chloride through saturated aqueous common salt, after concentrated sulphuric acid drying with Iod R in the glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution after, obtain the glacial acetic acid of lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution;
(3) regulate with the glacial acetic acid of the glacial acetic acid of iodine and the lodine chloride of methenyl choloride or phenixin or cyclohexane mixed solution and preparation and methenyl choloride or phenixin or cyclohexane mixed solution, regulate in the glacial acetic acid of afterchlorinate iodine and methenyl choloride or phenixin or cyclohexane mixed solution, the mol ratio of iodine and chlorine is 1:0.96 ~ 0.99, the iodine value reagent namely improved;
(4) reaction residue of preparation of chlorine is through process, and recovery obtains manganese dioxide and recycles.
The invention has the advantages that: react with certain fineness manganese dioxide and concentrated hydrochloric acid and prepare chlorine, the chlorine of preparation removes hydrogen chloride through saturated aqueous common salt, after concentrated sulphuric acid drying with Iod R in the glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution after, obtain the glacial acetic acid of lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution.Be unreacted manganese dioxide, manganous chloride in the reaction residue of preparation of chlorine, unreacted hydrochloric acid, obtains manganese dioxide, method environmental protection through process recovery.
Accompanying drawing explanation
Fig. 1 is preparation of chlorine of the present invention and logical chlorine device schematic diagram.
Embodiment
Schematic diagram is as shown in Figure 1 known, and device used in the present invention comprises pressure regulator 1, lifting table electric furnace 2, addition funnel there-necked flask 3, saturated common salt water filtering bottle 4, concentrated sulphuric acid drying bottle 5, iodine monochloride solution prepare bottle 6, vacuum buffer bottle 7, vacuum meter 8, vacuum breaker 9, vacuum pump 10 and tail gas absorption bottle 11.
The chemical reaction that the present invention uses is: preparation of chlorine reacts: MnO
2+ 4HCl=MnCl
2+ 2H
2o+Cl
2↑; Prepare the reaction of iodine monochloride solution: Cl
2+ I
2=2ICl, can occur if chlorine is excessive: ICl+Cl
2=ICl
3; Tail gas absorption: Cl
2+ 2NaOH=NaCl+ NaClO+ H
2o; Chemical reaction: MnCl is reclaimed in the residual process at night of preparation of chlorine
2+ 2NaOH=Mn(OH)
2↓+2NaCl, 2Mn(OH)
2+ O
2(oxygen in air)=2 MnO
2↓+2H
2o; Excessive unreacted hydrochloric acid NaOH neutralizes: HCl+NaOH=NaCl+ H
2o.
The following examples, with mixed solvent acetic acid and methenyl choloride for 4:1 volume ratio, all glass apparatus and pipeline want dried and clean, and concrete preparation method is as follows:
1. 65 grams of iodine are dissolved in the mixed solvent of 5000 milliliters of acetic acid and methenyl choloride, heating if desired promotes to dissolve, the iodine solution prepared leaves in 5000 milliliters of transparent white narrow mouth reagent bottles, shakes up, and pours out mol ratio that 500 milliliters of iodine solutions keep iodine below and chlorine and regulate and use after cooling;
2. manganese dioxide is ground, cross 100 mesh sieves, the rear 40 grams of manganese dioxide that will sieve to be put in 1000 milliliters of ground there-necked flasks 3, there-necked flask 3 flask holder is fixed on iron stand, prepare three supporting tool hole tetrafluoro plugs, interstitial hole is fitted with the addition funnel of concentrated hydrochloric acid 200 milliliters, other 2 mouthfuls one connects emptying glass piston valve, one connects chlorine gas outlet, the electric furnace 2 with lifting table transferred by flask 3, electric furnace 2 pressure regulator 1 controls heating, chlorine gas outlet is connected to 500 milliliters of saturated common salt water filtering bottle 4 entrances (in wash bottle anti-150 ~ 200 milliliters of additional 30 grams of salt of saturated aqueous common salt), saturated common salt water filtering bottle 4 outlet is received in 500 milliliters of concentrated sulphuric acid drying bottle 5(and is added 200 milliliters of concentrated sulphuric acids) entrance, concentrated sulphuric acid drying bottle 5 outlet is connected to iodine monochloride solution and prepares bottle entrance 6, iodine monochloride solution is prepared bottle outlet 6 and is connected to vacuum buffer bottle entrance 7, vacuum buffer bottle outlet 7 is by pipeline connecting tee, threeway one connects vacuum meter 8, other one connects an other threeway, second threeway one connects vacuum breaker 9, other one connects vacuum pump 10, vacuum pump 10 tail gas pipeline absorbs after except remaining chlorine through the NaOH in tail gas absorption bottle 11 and discharges.Each interface and rubber plug tetrafluoro raw material band is coated and sealing;
3. first close the emptying glass piston valve that flask 2 connects, open vacuum pump 10, vacuum meter 8 is regulated to be pressed between 0.005 to 0.02mpa with vacuum breaker 9, the too little chlorine that prevents of vacuum leaks, vacuum is too large, prevent the wijs reagent volatilization loss of preparation serious, part opens concentrated hydrochloric acid addition funnel, appropriate unlatching hot plate 2 heats, the chlorine of preparation is through purification, in the acetic acid passing into iodine after drying and methenyl choloride mixed solution, along with passing into of chlorine, the acetic acid of iodine and methenyl choloride mixed solution can react the acetic acid and methenyl choloride mixed solution that become lodine chloride, reactant liquor color slowly can change to dark brown red by pitchy is opaque, see that the glacial acetic acid of lodine chloride and the mixed solution of methenyl choloride turn down concentrated hydrochloric acid when deepening brownish red and add, during to salmon pink, close concentrated hydrochloric acid funnel, open emptying glass piston valve, close vacuum pump 10, open vacuum breaker 9.Logical chlorine is to iodine monochloride solution becomes salmon pink (at this moment chlorine/iodine is greater than 1 than micro-).Remove logical chlorine device, preparation of chlorine raffinate recycles, and prepares the proportion adjustment carrying out chlorine and iodine after the acetic acid of lodine chloride and methenyl choloride mixed solution return to room temperature.
The adjustment of iodine and chlorine ratio in the glacial acetic acid of lodine chloride and the mixed solution of methenyl choloride, regulate with reference to the concrete method for making of invalid patent CN1236101A Section three, be that 0.96 ~ 0.99:1 is advisable by the proportion adjustment of chlorine and iodine, under this ratio, iodine monochloride solution is the most stable, chlorine/iodine ratio can not be greater than 1, otherwise except addition reaction also substitution reaction may occur when measuring iodine number, increasing metrical error, only there is addition reaction in determination of iodine value lodine chloride and tested substance.
The iodine monochloride solution regulating chlorine/iodine ratio is transferred in the brown ground reagent of dried and clean, keeps in Dark Place, as detection iodine value reagent.
4. preparation of chlorine reaction residue process, pipettes the concentrated hydrochloric acid do not dripped, and can continue next time to use.Add 100 ml waters in there-necked flask, load onto stirring, under agitation regulate residue ph to 8 ~ 9 with the NaOH of 10%, suction filtration, washes filter residue with water, and filter residue is put in evaporating dish and dried, grinding, namely reclaims and obtains manganese dioxide, can be used as next group preparation of chlorine.
Claims (1)
1. a preparation method for the iodine value reagent improved, its concrete steps are as follows:
(1) glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution is prepared;
(2) chlorine obtained by certain fineness manganese dioxide and concentrated hydrochloric acid, the chlorine of preparation removes hydrogen chloride through saturated aqueous common salt, after concentrated sulphuric acid drying with Iod R in the glacial acetic acid of iodine and methenyl choloride or phenixin or cyclohexane mixed solution after, obtain the glacial acetic acid of lodine chloride and methenyl choloride or phenixin or cyclohexane mixed solution;
(3) regulate with the glacial acetic acid of the glacial acetic acid of iodine and the lodine chloride of methenyl choloride or phenixin or cyclohexane mixed solution and preparation and methenyl choloride or phenixin or cyclohexane mixed solution, regulate in the glacial acetic acid of afterchlorinate iodine and methenyl choloride or phenixin or cyclohexane mixed solution, the mol ratio of iodine and chlorine is 1:0.96 ~ 0.99, the iodine value reagent namely improved;
(4) reaction residue of preparation of chlorine is through process, and recovery obtains manganese dioxide and recycles.
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|---|---|---|---|
| CN201210479805.XA CN102944642B (en) | 2012-11-23 | 2012-11-23 | A kind of preparation method of iodine value reagent of improvement |
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| CN110577191A (en) * | 2019-08-20 | 2019-12-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for directly preparing iodine monochloride from iodine-containing salt |
| CN113387329A (en) * | 2021-07-16 | 2021-09-14 | 成都市科隆化学品有限公司 | Low-cost high-efficiency preparation method of iodine monochloride and obtained iodine monochloride |
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Non-Patent Citations (1)
| Title |
|---|
| 配制wijs液测定棕榈油碘价;李定一 等;《旅行医学科学》;19981231(第2期);第1.1节至第3节 * |
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