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Bi bo co ha Hu C 2

MC LC
Bi 1 ................................................................................................................................ 2
Bi 2 ................................................................................................................................ 3
Bi 3 ............................................................................................................................... 5
Bi 4 ............................................................................................................................... 7
Bi 5 ............................................................................................................................... 9
Bi 6 ............................................................................................................................. 14
Bi 7 ............................................................................................................................. 15
Bi 8 ............................................................................................................................. 16
Bi 9 ............................................................................................................................. 17

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Bi bo co ha Hu C 2

Bi 1:

TCH ACID, BASE V HP CHT TRUNG HA

I. QU TRNH THC HNH
1. Chit hn hp benzoic acid, napthalene v aniline
Cho 3 gam hn hp vo erlen 50ml v thm 30ml diethyl ether (ch
diethyl ether l cht d chy, khng gn la v ngun nhit), lc cho
n khi hn hp ng nht. Cho ton b hn hp vo phu chit, dng
ether trng erlen. Thm 10ml nc, thm tip 10ml dung dch HCl
3M. y np phu chit li. Lc phu chit 3 ln ri tho p sut, ri lm
tip tc nh th 3 ln th yn phu chit ln gi. Khi tch thnh 2 lp,
ly lp bn di vo erlen 50ml (nh du erlen ny l erlen A)
Cho tip 10ml dung dch NaOH 1,5M vo phu chit, lc nh trn,
ri yn ln gi, tch ly lp cht lng pha di cho vo erlen 25ml
(nh du erlen ny l erlen B). Thm tip 5ml nc vo phu chit, lc
hn hp, tch ly lp cht lng bn di cho vo erlen B
Lc ny mt lng ln nc cn trong lp trn (lp ether), ta c
loi b nc bng cch chit vi dung dch sodium chlorua bo ho. Cho
15ml dung dch NaCl bo ho vo phu chit, lc v yn, sau tch
b lp bn di. Cho lp trn vo erlen 50ml (nh du l erlen C).
Thm khong 1g Na2SO4 vo lc v lng
2. Thu hi sn phm
Base ho cht lng trong erlen A bng dung dch NaOH 8M cho
n khi pH >= 10. Sau lm lnh erlen A. Ghi nhn hin tng.
Acid ho erlen B bng 3ml HCl c, kim tra pH dung dch phi <=
2. Sau lm lnh erlen B. Ghi nhn kt qu
Lc ly dch lc ether trong erlen C. C quay thu hi dung mi
ether, thu ly sn phm cn li. Cn v ghi nhn gi tr khi lng
Kt tinh sn phm trong erlen A v B. Lc (bng phu Buchner) v
ra sn phm li bng nc lnh. Cn khi lng sn phm
II. KT QU THC HNH
Do ht qu cht trong qu trnh thc hnh nn th nghim khng hon thnh.

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Bi bo co ha Hu C 2

Bi 2:

PHN NG SULFO HA
I.

TIN HNH TH NGHIM

1. iu ch sodium p-toluenesulfonate
Trong erlen 250ml cho vo 10ml toluene, 10 ml H2SO4 c
Tin hnh un hon lu cho n khi lp toluene bin mt.
Ngng un, ngui erlen, cho hn hp ny vo becher 500ml c cha
sn 50ml nc. Trng bnh cu vi 1 t nc lnh v vo hn hp trn.
Thm tng lng nh tinh th sodium bicarbonate vo dung dch trn,
dng a thy tinh khuy u cho n khi dung dch ht si bt.
Tip tc thm vo 10g tinh th NaCl, khuy cho tan. Nu dung dch c
mu cho vo khong 1g than hot tnh. un si nh vo khuy u trong 10
pht.
Dng phu thy tinh lc nng sn phm.
Lm lnh dung dch qua lc, sn phm s kt tinh.
Lc kh sn phm di p sut km.
2. Kim tra ha tan ca sodium p-toluenesulfonate
Kim tra ha tan ca sodium p-toluenesulfonate trong ethanol, acetone
v nc.

II.

KT QU TH NGHIM
1. iu ch sodium p-toluenesulfonate
iu ch thnh cng sn phm sodium p-toluenesulfonate nhng trong
qu trnh lm th nghim, phng th nghim khng c lc chn khng nn
gp kh khn trong vic lc, ch lc thng.
2. Kim tra ha tan ca sodium p-toluenesulfonate
Sodium p-toluenesulfonate tan nhiu trong nc, tan nhiu trong ethanol
nhng t hn trong nc v tan t trong acetol.

III. TR LI CU HI CNG C
1. C ch phn ng

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Bi bo co ha Hu C 2

2. Hiu sut phn ng

Do khng th cn sn phm nn khng th tnh hiu sut ca phn ng.
3. Tc dng ca sodium bicarbonate
Sodium bicarbonate c tc dng trung ha acid H2SO4 d, tham gia to mui vi
acid para-tolunen sufonic, to mun para-tolunen sufonat natri.

4. Tc dng ca NaCl

Tc dng ca NaCl to ra Na+ to ion chung, lm tng kh nng to mui.

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Bi bo co ha Hu C 2

BI 3:

PHN NG X PHNG HA
I. CCH TIN HNH
1. iu ch x phng
un hn hp du thc vt v
ethanol cho n khi hn hp ng
nht

Thm NaOH vo hn hp phn

ng v un n khi dd trong sut
hn hp vo dd NaCl bo ha
Xut hin kt ta

Lc ly x phng, cn ghi nhn

khi lng x phng.

2. Kim tra tnh cht ca x phng

a. Chun b dung dch x phng
- Chun b 2 cc:
+ Cc 1: 1 gam x phng va iu ch c + 50ml nc
+ Cc 2: 1 gam x phng trn th trng + 50ml nc
b. Kim tra tnh cht x phng
- Kim tra pH: dng a thy tinh khuy u mi cc sau chm vo giy pH, ghi nhn
gi tr pH.
- Kim tra s to bt: thm vo 2 ng nghim, ng 1 dung dch x phng va iu ch
c v ng 2 dung dch x phng thng mi. Dng ngn tay bch u ng nghim li
v st trong 10 giy. Quan st s to bt trong mi ng nghim.
- Tng tc vi du: thm vo 2 ng nghim mi ng 5 git du. Dng ngn tay bch u
ng nghim v st trong 10 giy. Quan st lp du trong mi ng nghim. Ghi nhn
lng bt, so snh vi th nghim kim tra s to bt.
- Kim tra vi nc cng: thm 20 git CaCl2 1% vo 2 ng nghim. Dng ngn tay bch
u ng nghim v st trong 10 giy. Quan st lp du trong mi ng nghim. Ghi nhn
lng bt, so snh vi th nghim kim tra s to bt.

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Bi bo co ha Hu C 2

Thm 20 git MgCl2 1% vo 2 ng nghim. Dng ngn tay bch u ng nghim v st

trong 10 giy. Quan st lp du trong mi ng nghim. Ghi nhn lng bt, so snh vi
th nghim kim tra s to bt.
Thm 20 git FeCl3 1% vo 2 ng nghim. Dng ngn tay bch u ng nghim v st
trong 10 giy. Quan st lp du trong mi ng nghim. Ghi nhn lng bt, so snh vi
th nghim kim tra s to bt.

II. KT QU TH NGHIM
1. iu ch x phng
To ra sn phm nh mong mun. Nhng khng c kt tinh li sn phm tinh
c ch thu c sn phm th do khng c lc p sut.
Khi lng sn phm th: mth = 44,638 1,465 = 43,173
2. Kim tra tnh cht ca sn phm
a. Kim tra pH:
pH ca x phng iu ch c = 9
pH ca x phng trn th trng = 10
Gn ging vi x phng trn th trng
b. Kim tra s to bt, tng tc vi du, kim tra vi nc cng
So snh s to bt ca x phng trong cc trng hp trn, ta nhn thy s to bt
ca x phng va iu ch c thp hn x phng trn th trng.
Nguyn nhn do x phng bn trn thj trng c cho thm cht to bt trong qu
trnh sn xut.

III. TR LI CU HI CNG C
1. Tnh hiu sut phn ng:
2. Vit c ch phn ng x phng ha
Phng trnh phn ng:

c ch phn ng:

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Bi bo co ha Hu C 2

BI 4:

PHN NG GHP CP
I. TIN HNH TH NGHIM
1. iu ch acid sulfanilic
un hn hp gm 10ml aniline v 20ml sulfuric acid bng h thng sinh hn
nhit 1800C trong 1 gi 40 pht. Phn ng kt thc nu ha tan 1 git hn hp
vo 4ml NaOH 10% thy tan hn. ngui, lm lnh v lc sn phm
tinh ch, cho acid th vo cc thm 75ml nc un n 800C trn ni cch
thy, thm tng git NaOH n khi tan hon ton, thm 0,5 gam than hot tnh,
tip tc un v lc nng. Acid ha phn dd lc bng HCl. Lm lnh v lc phn
kt ta. Cn khi lng sn phm thu c.
2. Diazo ha sulfanilic acid
Ha tan 2 gam sulfanilic acid vo 4,5 ml dung dch NaOH 10% trong beaker
thy tinh c dung tch 100ml ( c th un nh n khi tan hon ton). Pha long
dung dch bng 15 ml nc, va khuy va cho 4,5 ml axit sunfuric c vo. Lm
lnh ton b hn hp phn ng n 0-5oC. Va khuy, va nh t t dung dich
gm 1g sodium nitrite trong 5ml nc. Trong qu trnh cho dung dch sodium
nitrite cn kim tra axit ca mi trng (pH = 1-2) v gi nhit phn ng t
10-13 oC. Khi thm gn ht dung dch sodium nitrite cn kim tra s kt thc ca
phn ng diazo ha bng giy KI/h tinh bt (xem phn tng hp phenol). Sn
phm tch ra dng bt trng l mui iazoni ca p-diazobenzenssulfonic acid
dng ion lng cc.
Trung ha dung dch mui diazonium ca sulfanilic acid bng dung dch
Na2CO3 10% n pH=4-5.
3. Phn ng ghp cp iu ch -naphtol da cam
Ha tan mt beaker khc dung tch 250ml 1,8 gam - naphtol trong 6ml
dung dch NaOH 10%. un nng nh - naphtol tan hon ton, thm vo
20ml nc v lm lnh ton b dung dch n 10 oC.
Sau khuy dung dch - naphtolate lnh va cho dung dch mui iazoni
lnh vo, ng thi gi nhit ca hn hp phn ng 0 - 5oC. Trong qu trnh
phn ng ghp i cn duy tr mi trng ca hn hp phn ng l mi trng
kim yu (pH = 8,8-9). Trng hp pH thp hn cn iu chnh bng dung dch
NaOH 10%, kt thc phn ng hn hp cn phi d mt t - naphtolate.
Khuy hn hp phn ng thm 15 pht na hon thnh phn ng ghp i.
Sau ton b khi phn ng c un trn ni cch thy 60 oC c mt
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dung dch ng th. Lc nng dung dch v cho vo dung dch 15g NaCl, khuy
u v lm lnh bng . Sau mt thi gian kt ta s tch ra, lc ly sn phm
bng phu buchner, p kh v kh ngoi khng kh.
Sn phm c kt tinh li bng nc ethanol: ha tan sn phm th vi mt
lng va nc si, lc nng, dch lc ngui dn n 70 - 80 oC, cho thm
vo 10ml ethanol v lm lnh hn hp, sn phm s tch ra di dng tinh th
mu da cam.
II. KT QU THU C
1. iu ch acid sulfanilic
iu ch c sn phm dng th. Nhng khng th cn khi lng do trong
qu trnh sy sn phm, sn phm b nng chy.
Nguyn nhn: khi sy dng c th nghim cc bn khc chnh nhit qu cao
lm cho sn phm b nng chy.
2. Diazo ha sulfanilic acid
Sn phm thu c c mu da cam.
3. Phn ng ghp cp iu ch -naphtol da cam
C iu ch thnh cng nhng khng cn c sn phm.

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Bi bo co ha Hu C 2

Bi 5:

IU CH NHA PHENOL FORMALDEHYDE

TIN HNH TH NGHIM

I.

Cn ng nghim.
Cn 14.10 g phenol cho vo becher (h nng khong 70oC phenol ho lng
ri cn). Sau thm 2,00ml nc, 9.00 ml dung dch formalin 37% cho vo. Cui
cng thm vo 1ml HCl 5M.
* Ch : Ly lng phenol v formaldehyd phi tht chnh xc.
Khuy u hn hp sau y becher bng giy parafine, lm thng 1 l nh
trn mt. quan st hin tng, un nh 50oC. Khi hn hp phn ng bt u c v
tch thnh 2 lp th sau 10 pht dng a thy tinh ly 2g nha, ra nhiu ln bng
nc, cui cng trng aceton ri o nht. Sau ly thm 2 mu na thi gian
cch nhau gia cc mu l 20 pht.
Hn hp nha cn li sau khi loi ht nc th tip tc gia nhit cho n khi
ng rn hon ton, ngui quan st mu sc ca nha v gii thch hin tng.
* o nht bng nht k Ostwald:
Cn 2.0 g nha ca mi mu vo erlen nh cha 8.0 g ethanol tuyt i. Khuy
tht k cho nha tan ht vo trong dung dch.
u tin o nht dung mi (ethanol tuyt i-to), sau o dung dch nha.
(t). Mi dung dch o t nht 3 ln.
Tnh nht tng i ca mu nha []td = t/ to
Xc nh nht rt gn []rg, nht c trng [],[] l gii hn ca rg
khi nng lng C ca dung dch tin ti 0. Gi tr [] c xc nh thng qua
th. Suy ra khi lng phn t trung bnh nht ca polymer bng cng thc :

[] = K. M v a
II.

KT QU TH NGHIM

SN PHM

nht
Ln 1

Ln 2

Ln 3

Ethanol

2p14s

2p12s

2p11s

Sn phm 1

5p1s

5p0s

4p50s

Sn phm 2

4p52s

4p52s

4p52s

Sn phm 3

4p40s

4p33s

4p35s

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SN PHM

Bi bo co ha Hu C 2
nht tng i = t/t0
Ln 1

Ln 2

Ln 3

Sn phm 1

2,25

2,27

2,21

Sn phm 2

2,18

2,21

2,23

Sn phm 3

2,09

2,07

2,10

SN PHM

nht ring
Ln 1

Ln 2

Ln 3

Sn phm 1

1,25

1,27

1,21

Sn phm 2

1,18

1,21

1,23

Sn phm 3

1,09

1,07

1,10

SN PHM

nht rt gn
Ln 1

Ln 2

Ln 3

Sn phm 1

2.08

2.11

2.02

Sn phm 2

1.97

2.02

2.05

Sn phm 3

1.82

1.78

1.83

III. CU HI CNG C
C ch phn ng:

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Bi bo co ha Hu C 2

1. C th iu ch nha novolac tan c t recorcinol khng?

Recorcinol l mt trong nhng dn xut ca phenol vi 2 nhm hydroxy v
tr 1 v 3 ca vng benzene do vy tnh cht ha hc ca recorcinol c nhng
im tng ng vi phenol.

Khng th iu ch nha novolac tan c t recorcinol. Bi v recorcinol c 2

nhm OH ( Benzen1,2-diol) nn mc linh ng ca H ti othor v para khng bng
phenol.
Di y l phn ng to nha novolac t phenol:

Ion metylol s tn cng vo v tr giu in t ca phenol.

Trong mi trng axit cc metylol phenol khng bn, chng tng tc vi ion
H+ to ion metylolphenol.
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Bi bo co ha Hu C 2

2. Ti sao nha Bakelite lu ngoi khng kh thng hay c mu sm?

Nha Bakelite tng hp c t phenol, m iu kin thng phenol tn ti

dng tinh th hnh kim, khng mu, c mi hc c trng, lu trong khng
kh c mu hng v bin thnh mu nu nht do n b oxi ho.

3. Ti sao cn phi thm hexamethylenetetramine to thnh hp cht

Novolac c th c khun c (Novolac molding compound)? C th s
dng 1 amine khc hay khng?
Hexamethylenetetramine l mt hp cht hu c d vng vi cng thc
(CH2) 6 N 4. Trng ny tinh th hp cht ha tan cao trong nc v cc dung
mi hu c cc. N c cu trc ging nh ci khung tng t
nh adamantane . N rt hu ch trong vic tng hp cc hp cht ha hc
khc, v d nh nha, dc phm, ph gia cao su. N thng hoa trong chn
khng 280 C.
iu ch nha novolac ngoi formaldehyde v aldehyde khc c th
dng hexa metylentetra amin, khi un nng phenol vi urotropin ( trong mi
trng ru) vi t l 1,2 :1 th nhn c nha novolac cha nit, c th
dng nhm dimetylen amin (-CH2-NH-CH2-), phn ng ny ta ra NH3.
Nu un nng nha novolac v nha i t phenol c thay th gc alkyl v tr
octo v para 200-280oC th chng c kh nng chuyn sang trng thi khng
nng chy khng ha tan, v nhm hydroxyl ca phenol tham gia vo vic to
ra lin kt ete.
Do nhng trung tm phn ng t do ca nha novolac ( v tr octo v
para so vi nhm hydroxyl ca nhn phenol) lm cho nha ny c kh nng
chuyn sang trng thi khng nng chy, khng ha tan khi cho tc dng vi
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Bi bo co ha Hu C 2

formaldehyde hoc urotropin. ng rn nha novolac c km theo hin tng

to ra nhm metylen v nhm dimetylenimin.

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Bi bo co ha Hu C 2

BI 6
IU CH V LM TINH KHIT ESTER ETHYL ACETATE
I.

C s l thuyt
Ester l mt nhm chc c COO- , c th c tng hp t cacboxylic
acid v ru vi xc tc l acid H+
Phn ng ester ha l phn ng cn bng, c hng s cn bng K c
=4 nhit phng:
C2H5OH + CH3COOH

II.

III.

CH3COOC2H5 + H2O
Ethyl acetate
Ethyl acetate ( EA) l este ca ethanol v acid acetic vi cng thc CH3COO-CH2-CH3. Cht lng khng mu ny c mi ngt c trng v c s
dng trong keo dn. Ethyl acetate c s dng ch yu nh mt dung mi
v cht pha long, c a chung v chi ph ca n thp, c tnh thp, v
mi d chu.
Tin trnh th nghim
1. iu ch ethyl aceiate
Cho 10ml ethanol + 12ml acetic acid +15 git H2SO4.
un cch thy 40 pht v ngui.
Ta c hn hp este v nc
2. Tch este
4,5 g Na2CO3 + 15ml nc ct.
Cho dd Na2CO3 bo ha + hn hp phn ng vo phu chit
Ly lp ethyl acetate pha trn cho vo bnh cu.
3. Tinh khit ester
Ly bnh cu cha ethyl acetate, lp h thng chng ct.
Cn erlen hng ester.
Chng ct n khi cht lng trong bnh cu cn li rt t.
Cn li erlen v ghi khi lng
Kt qu th nghim

Khi lng sn phm thu c: m= 3,9g.

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Bi bo co ha Hu C 2

BI 7
PHN NG ALKYL HA IU CH ETER
I.

NAPHTYL ETYL

C s l thuyt
O
C
R vo phn t hp cht
Phn ng alkyl ha l qu trnh gn nhm
hu c, thng bng phn ng th hydro ca hydrocarbon thm v hydro
ca mt vi nhm chc.
Trong tng hp hu c, phn ng quan trng l alkyl ha hydrocarbon
thm theo c ch SE.
Phng trnh phn ng:

OC2H5

OH
H+

+ C2H5OH

II.

+ H2O

Tin trnh th nghim

Cho 15 gam - naphtol + 20ml ru etylic (lc k)
Thm vo 3ml H2SO4 (ung trong 2 gi).
Cho 45 ml dung dch NaOH 5% un nng ln 50oC . Khuy mnh cho
hn hp tan ht. Cht kt ta c mu vng nu.
Lc v x l ln na bng dd NaOH 5%. Ra sn phm bng nc n khi
giy qu khng i mu.
Sy sn phm nhit 450C.

III.

Kt qu th nghim
Khi lng sn phm thu c : mtt = 12.57g
Khi lng theo l thuyt : mlt =17.9
H=
= 70.22%.

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Bi bo co ha Hu C 2

BI 8
PHN NG OXI HA TOLUENE
I.

C s l thuyt
Toluen, hay cn gi l mtylbenzen hay phenylmtan, l mt cht lng
trong sut, khng ha tan trong nc.
Phn ng c chia lm 2 giai on:
Giai on 1:
CO O K

CH3
+ K M nO 4

+ KOH +

M nO 2 +

H2O

Giai on 2
COOH

COOK
+ HCl

II.

KCl

Tin hnh th nghim

Cho 5ml toluen + 5g KMnO4. un hn hp trong 2 gi (un hon lu).
Thm vo 3ml H2SO4 c + vi git ethanol
Lc b mangan dioxit
un cch thy khi th tch cn 25ml
Acid ha bng dung dch HCl.
Lm lnh bng . Lc bng nc lnh. Thu sn phm

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Bi bo co ha Hu C 2

BI 9
IU CH 4 BROMOAMNILINE
I.

C s l thuyt
Aniline tham gia phn ng th thn in t trn nhn thm mnh do hiu
ng cng hng trong phn t, lm mt electron trn nhn thm tng.
Aniline phn ng vi bromine to sn phm th poly l 2,4,6
tribromoaniline .
NHAc

NH2

NHAc

Ac2O

Br2

AcOH

AcOH

NH2
i. HCl
ii. NaOH

Br

II.

Br

u tin aniline c chuyn thnh acetanilide, sau bromo ha to

sn phm v tr 4 Sau khi bromo ha, nhm amide b thy phn to li
nhm amine
Tin hnh th nghim
1. iu ch acetanilide ( N phenylethanamide)
Cho 25ml acetic acid + 10ml aniline + 12ml acetic anhydride. Khy diu
v ngui trong 5 pht
Thm t t 100 200 ml nc cho ti khi xut hin kt ta
Lc ly tinh th.
Kt tinh li bng ethanol
2. iu ch N ( 4 brom phenyl ) ethanamide ( p-bromoacetanilide ):
Cho 25ml acetic acid vo trong acetanilide.
Ha tan bromine vo 25ml acetic acid.
Trn chung hn hp li vi nhau.
Khy u v ngui khong 15 pht them 30ml nc ct, lc ly sn
phm
3. iu ch 4 bromoaniline:

III.

Cho N ( 4 brom phenyl ) ethanamide + acid HCl. un hn hp trong

10 pht sau lm ngui (un hon lu cho ti khi hn hp tan ht ).
ngui khong 5 pht
dung dch bromine vo dung dch acetanilide. Kim ha bng NaOH.
Lm lnh v lc ly sn phm
Kt qu th nghim
Khi lng sn phm th= 12.92g
Khi lng giy lc =0.6791g
Khi lng sau kt tinh=9.066g

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